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Method for large-batch separating preparation of high-purity theaflavine monomer

A large-scale separation and high-purity technology, applied in organic chemistry and other directions, can solve the problems of poor separation selectivity, difficult purification, and difficulty in the separation of high-purity theaflavin monomers in large quantities. Effect

Inactive Publication Date: 2007-12-05
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the above four main theaflavins, in general, TF and TFDG are relatively easy to separate from other theaflavins, while the separation between the two TF-MGs has been very challenging. Only a partial separation of it can be achieved using any of the above methods
For the purpose of mass preparation and separation, as the amount of sample loaded increases, the separation selectivity of the two will be worse, and the purification will be more difficult
Therefore, the large-scale separation of high-purity theaflavin monomers has always been difficult

Method used

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  • Method for large-batch separating preparation of high-purity theaflavine monomer
  • Method for large-batch separating preparation of high-purity theaflavine monomer
  • Method for large-batch separating preparation of high-purity theaflavine monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1: The first step of column chromatography separation of theaflavin crude extract (referring to the flow chart of Fig. 1) takes black tea crude extract 40g, after dissolving with 70ml eluent, put on gel chromatographic column 1 (Sephadex LH- 20,900g, 100×10cm i.d.) for separation. Absolute ethanol was used as the eluent, and the average flow rate was 18ml / min. According to the color segment on the gel column after sample loading, collect in segments. After HPLC detection, the collected fractions were combined into three sections and 7 fractions, namely F0 mainly containing TF, F1, F2, F3, F4 containing TF-3-MG and TF-3'-MG, F5 (in order of elution), and the F6 fraction mainly containing TFDG. Figure 2 shows the HPLC analysis spectra of the Sigma mixed standard sample and the crude extract of theaflavins at two wavelengths. Analytical conditions: chromatographic column: Waters Xterra RP-C18 column (5 μ m, 150 * 4.6mm i.d.); Mobile phase: acetonitrile-water (28...

Embodiment 2

[0036] Example 2: Further isolation and purification of TF-3'-MG fraction

[0037] The TF-3'-MG relative content obtained by the separation of the crude sample is more than 50% F2, and the F3 fraction is put on a gel column for secondary separation respectively, and the column chromatography conditions adopted are the same as in Example 1. In the obtained fractions, the TF-3'-MG content in the 50%-90% fractions were separated by column chromatography for the third time. In this separation, 35%-acetone aqueous solution was used for elution. At this time, TF-3-MG The elution order of TF-3'-MG is opposite to the elution order of ethanol, TF-3-MG comes first, and TF-3'-MG comes after, so that more pure TF- 3'-MG. Three fractions A1 (7.83g), A2 (7.89g) and A3 (6.93g) with a relative content of TF-3'-MG obtained by repeated column chromatography separation and enrichment of more than 90% (wherein FL grade Fractions were combined with similar fractions) were further purified with H...

Embodiment 3

[0040] Example 3: Further isolation and purification of the TF-3-MG fraction

[0041] Combine the F4 and F5 with a relative content of TF-3-MG above 50% obtained from the separation of the crude sample and the similar fractions after the above-mentioned separation of TF-3'-MG. Fractions with a relative content of TF-3-MG of 50%-90% were separated by column chromatography for the third time, and the column chromatography conditions used were the same as those in Example 1. Grades B1 (0.52g) and B2 (17.27g) obtained by repeated separation and enrichment with a relative content of TF-3-MG above 90% were further purified by HSCCC to remove polar impurities therein.

[0042] Through HPLC analysis (as shown in Figure 7), it can be seen that B1 contains about 90% TF-3-MG and 10% TF-3'-MG; while B2 mainly contains TF-3-MG, TF- The 3'-MG content is very low, but contains a large amount of polar impurities in every fraction. Figure 8 shows the HSCCC separation spectrum of the B2 fract...

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Abstract

The present invention discloses process of separating black tea extract to prepare four kinds of high purity theaflavin and its derivatives in batch. By means of combining gel column chromatographic separation with great treating quantity and high speed countercurrent chromatographic separation with high separating efficiency, four kinds of theaflavin and its derivatives, including theaflavin (TF), theaflavin-3-gallate (TF-3-MG),theaflavin-3'-gallate (TF-3'-MG) and theaflavin-3, 3'-gallate (TFDG), in high purity are prepared. The process has great preparation amount, high product purity, short period, low solvent consumption and other features.

Description

technical field [0001] The invention relates to a method for separating and preparing high-purity theaflavin monomers in large quantities from black tea extracts. technical background [0002] Theaflavins (TFs) are a unique class of polyphenolic polymers in black tea, which are oxidized and polymerized by a pair of suitable catechins during the fermentation process of black tea. The content of theaflavins in black tea is very low, accounting for about 2% of dry weight, but they have a very important impact on the color and taste of black tea. Studies in recent years have shown that theaflavins not only have a great impact on the quality of black tea, but more importantly, it has a variety of biological activities closely related to human health, such as anti-cardiovascular disease, anti-virus, anti-inflammatory, anti- Oxidation, anti-tumor effect, etc. At present, there are more than a dozen kinds of theaflavins found in black tea, the main four of which are the following ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/74
Inventor 曹学丽董银卯黄丹凤李攀李挺
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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