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Method for extracting epigallocatechin gallate from oil-tea-cake

A technology for epigallocatechin and gallate, which is applied in the field of extraction of epigallocatechin gallate, can solve the problems of extracting EGCG that have not been seen before, and achieve low production cost, simple and easy-to-control process, and low dosage Effect

Inactive Publication Date: 2012-07-25
GUILIN SANBAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the raw materials for extracting EGCG are basically tea leaves, tea extracts or tea polyphenols, and there is no report on extracting EGCG from camellia oleifera cake

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) Crush the camellia oleifera cake to 10 meshes, take 50kg, soak in 200kg of petroleum ether at room temperature for 4 hours, filter with suction, collect the filter cake, and air-dry naturally at room temperature;

[0027] 2) Soak the air-dried filter cake with 60kg of ethyl acetate at room temperature for 24 hours, transfer it to the percolation cylinder, compact it, and then use 300kg of ethyl acetate for percolation extraction. The percolation speed is 1.5BV / h, and the percolation time For 5 hours, the percolation solution was concentrated under reduced pressure at 40°C, left to cool to room temperature, and the insoluble matter was removed by suction filtration, and the filtrate was collected;

[0028] 3) The filtrate is passed through the HPD-600 macroporous resin column, the flow rate of the column is 1.5BV / h; the resin column is washed with water until the effluent is colorless, the flow rate is 2.0BV / h, and then eluted with 30% (v / v) ethanol, the flow rate is 1...

Embodiment 2

[0034] 1) Crush the camellia oleifera cake to 20 mesh, take 100kg, soak it in 300kg6# solvent oil at room temperature for 5h, filter with suction, collect the filter cake, and air-dry naturally at room temperature;

[0035] 2) Soak the air-dried filter cake with 100kg 60% (v / v) ethanol at room temperature for 24 hours, transfer it to the percolation cylinder, compact it, and then extract it with 500kg 60% (v / v) ethanol percolation, the percolation speed The percolation time is 1.0BV / h, the percolation time is 4h, the percolation solution is concentrated under reduced pressure at 40°C, left to cool to room temperature, and the insoluble matter is removed by suction filtration, and the filtrate is collected;

[0036] 3) The filtrate is passed through NKA-9 macroporous resin column, the flow rate of the column is 1.0BV / h; the resin column is washed with water until the effluent is colorless, the flow rate is 2.0BV / h, and then eluted with 25% (v / v) ethanol, the flow rate is 1.0 BV...

Embodiment 3

[0042] 1) Crush the camellia oleifera cake to 10 meshes, take 10kg, soak in 100kg of 6# solvent oil at room temperature for 3 hours, filter with suction, collect the filter cake, and air-dry naturally at room temperature;

[0043] 2) Soak the air-dried filter cake with 30kg 70% (v / v) methanol at room temperature for 24 hours, transfer it to the percolation cylinder, compact it, and then extract it with 50kg 70% (v / v) methanol percolation. The percolation time is 2.0BV / h, and the percolation time is 3.5h. The percolation liquid is concentrated under reduced pressure at 40°C, left to cool to room temperature, and the insoluble matter is removed by suction filtration, and the filtrate is collected;

[0044] 3) Pass the filtrate through the S-8 macroporous resin column with a flow rate of 1.0BV / h; wash the resin column with water until the effluent is colorless at a flow rate of 1.0BV / h, then elute with 20% (v / v) ethanol at a flow rate of 0.8 BV / h, thin-layer chromatography tracki...

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PUM

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Abstract

The invention discloses a method for extracting epigallocatechin gallate from oil-tea-cake. The method comprises the following steps of: (1) smashing an oil-tea-cake as a raw material, adding a solvent to carry out percolation extraction, collecting percolate, recovering the solvent, filtering and collecting filtrate; (2) feeding the filtrate for macroporous resin column chromatography, eluting the column by using 20-30% (v / v) of ethanol after rinsing the column, tracking and detecting by utilizing thin-layer chromatography and collecting ethanol eluent; (3) concentrating the ethanol eluent, adding organic acid into the concentrated solution, standing to crystallize; (4) dissolving the obtained crystals by using a mixed solvent 1, carrying out silicagel column chromatography, firstly washing the column by utilizing the mixed solvent 1, then washing the column by utilizing a mixed solvent 2 and collecting the eluent of the mixed solvent 2; and (5) concentrating the eluent obtained in the step (4), adding the organic acid and a little high-purity epigallocatechin gallate into the concentrated solution, standing, crystallizing, drying the crystals to obtain. The method disclosed by the invention has the advantages that the process is simple and easy to control; the eluent consumption is little; the yield is high and the production cost in low.

Description

technical field [0001] The invention relates to a method for extracting epigallocatechin gallate, in particular to a method for extracting epigallocatechin gallate from camellia oleifera cake. Background technique [0002] Camellia oleifera cake is a cake-like residue pressed from the seed kernels of Camellia oleifera Abel, an evergreen tree of the genus Camellia oleifera in the family Theaceae. Camellia oleifera cake contains fat, protein, crude fiber, tea saponin, sugar and a small amount of polyphenol antioxidant active substances, from which residual oil, tea saponin, polyphenols and other substances can be extracted. As a natural antioxidant, polyphenol has the characteristics of strong antioxidant capacity and good safety. It is a natural antioxidant worthy of further research and development, especially epigallocatechin gallic acid, which has the strongest antioxidant properties EGCG, which has anti-oxidation, anti-cancer, anti-mutation and other activities, the anti...

Claims

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Application Information

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IPC IPC(8): C07D311/62
Inventor 谢冬养谢阳姣卢照凯卢桦香应启实周晓青
Owner GUILIN SANBAO PHARMA
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