CN101921253B - Method for extracting epigallocatechin gallic acid ester from oolong tea by chromatography and membrane technology - Google Patents
Method for extracting epigallocatechin gallic acid ester from oolong tea by chromatography and membrane technology Download PDFInfo
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- CN101921253B CN101921253B CN2010101782510A CN201010178251A CN101921253B CN 101921253 B CN101921253 B CN 101921253B CN 2010101782510 A CN2010101782510 A CN 2010101782510A CN 201010178251 A CN201010178251 A CN 201010178251A CN 101921253 B CN101921253 B CN 101921253B
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Abstract
The invention relates to a method for extracting epigallocatechin gallic acid ester from oolong tea by chromatography and membrane technology. The method comprises the following steps of: (1) extracting tea liquid from oolong tea leaves with water; (2) carrying out membrane filtration and membrane concentration for removing impurities and decoloring to obtain purer tea polyphenol liquid; (3) carrying out chromatographic separation for separating catechin solution from the polyphenol liquid; (4) separating by using a polymeric membrane at room temperature to obtain EGCG solution; (5) concentrating the EGCG solution in vacuum and crystallizing to obtain EGCG crystal; and (6) freezing and drying the EGCG crystal to obtain a white solid EGCG product. The method has the advantages of low production cost, high product yield, high product purity of 98%, no residues and the like and is convenient for industrialized promotion.
Description
Technical field
The present invention relates to a kind of from oolong tea the method for extracting epigallocatechin gallic acid ester (hereinafter to be referred as EGCG), be a kind of method that adopts chromatography and membrane separating method separation and purification NVP-XAA 723 from oolong tea specifically.
Background technology
Tea-polyphenol is a kind of natural polyphenol class active substance that from tealeaves, extracts; It is major ingredient and effective ingredient EGCG, have the radical of removing, anti-oxidant, radioprotective, antitumor, antiviral, reducing blood-fat and SUV, antibiotic, plurality kinds of health care and pharmacological action such as delay senility.At present, the EGCG monomer has been classified as a kind of PTS that replaces taxol.Because mainly containing effective constituent in the tealeaves is tea-polyphenol; At present, EGCG is mostly extracted and is made by tealeaves, to this; The patent documentation that like Patent Office's publication number is CN101381359A just discloses " a kind of method of from green tea, extracting high-purity epigallocatechin-3-gallate "; Through with liquid-phase extraction method and the coupling of flicker silica gel column chromatography, make epi-nutgall catechin gallic acid ester monomer, though this method can make the high purity EGCG monomer; But owing to have complicated operation, big, the problems such as yield is low, loss is big, poisonous organic solvent (like chloroform) is residual, metal residual of investment, make product embarrass industries such as healthcare products and medicine to accept on the one hand; On the other hand; Research shows; Effective ingredient tea-polyphenol in the tealeaves of oolong tea, catechin monomers thing NVP-XAA 723 (EGCG) are higher nearly ten percentage points than green tea, therefore, from green tea, extract EGCG and compare oolong tea and do not have better resources advantage.
Summary of the invention
The objective of the invention is to provide a kind of new EGCG monomeric process for extracting, promptly adopt chromatography and membrane technique from oolong tea, to extract purifying EGCG and reach high yield, high purity and noresidue and be applicable to the purpose of industrialization.
For realizing above-mentioned purpose; The technical scheme that the present invention adopts mainly is to utilize the tea-polyphenol class of oolong tea and the difference of other impurity solubleness in solvent; Obtain the Polyphenols raw product with membrane filtration, membrane-concentrated impurity elimination respectively, utilize the chromatographic separation technology to make with extra care out tea-polyphenol again, reclaim organic solvent; Utilize membrane separation technique from the tea-polyphenol class, to isolate catechin EGCG monomer at last, and can get catechin EGCG product through crystallization and lyophilize.The method of implementing this scheme comprises the steps:
(1) extract, with oolong through water carry tea liquid.
(2) membrane filtration membrane-concentrated under the normal temperature, adopts the organic polymer rolled film to carry out removal of impurities and discolors, and TPS is removed in continuous extraction again, must purer tea-polyphenol appearance liquid.
(3) chromatographic separation, selecting volume for use is 2500cm
3, height is 70～100cm pillar, inserts polar resin; Mean particle size is inserted pillar with appearance liquid again about 50 orders, utilize resin absorption catechin component, removes impurity such as theine, pigment, and flow velocity is 1～2BV/h; Effluent is shoaled by scarlet; The water that adds 1～2BV amount cleans, and flow velocity is constant, is colourless to effluent; Using 1～2BV, concentration is that 70～80% ethanolic soln carries out desorb, and flow velocity is constant, collects coloured effluent, and this effluent is a catechin solution.
(4) membrane sepn under the normal temperature, pumps into catechin solution in the membrane separation plant, adopts polymeric membrane to separate, and the collection liquid after the separation is EGCG solution.
(5) crystallization is carried out vacuum concentration with EGCG solution, and temperature is 50 ℃～70 ℃, the EGCG liquid concentrator is placed crystallization under 5～10 ℃ of environment after making its solid content be increased to 25-45%, wait crystallization fully after, rinsing gets the EGCG crystal.
(6) lyophilize gets white solid EGCG product with the lyophilize of EGCG crystal.
The described polymeric membrane of above-mentioned steps (4) is a ceramic membrane, and the molecular weight that dams is 450～460.
Above-mentioned steps is carried out vacuum concentration with EGCG solution described in (5), and preferred temperature is 60 ℃, and preferred solid content is increased to 30%.
The present invention adopts technique scheme compared with prior art; Have the following advantages: first; Adopt membrane filtration and cryogenic film concentration technique to remove impurity such as fiber in the extracting solution, protein, pectin, solved fiber in the traditional technology, protein, pectin etc. effectively and be difficult to the problem of removing.Second; Utilize other component in the membrane separation technique dynamic separation tea-polyphenol; Solved the problem of the easy oxidation that product causes at traditional technology Yin Gaowen preferably; Overcome high energy consumption, height is consuming time, the product loss is high defective, production cost is low, yield is high, product purity reaches more than 98%, is easy to Industry Promotion.The 3rd, do not use poisonous organic solvents such as chloride, have the advantage of noresidue; Nor the use soda acid has more environmental protection.The 4th, the technological design flow process is scientific and reasonable, operates simple and easyly, and the EGCG monomer content of preparation reaches more than 98%, and product meets food safety requirements.
Embodiment
Embodiment 1:
1) extracts, oolong water liquid is carried out water carry and obtain tea liquid.
2) membrane filtration membrane-concentrated under the normal temperature, adopts the organic polymer rolled film to carry out removal of impurities and discolors, and TPS is removed in continuous extraction again, must purer tea-polyphenol appearance liquid (TP >=98%, EGCG >=50%).
3) chromatographic separation: with 100ml tea-polyphenol appearance liquid, its tea-polyphenol component is about 10g, at normal temperatures and pressures, the tea-polyphenol solution pump is gone in the resin adsorption column resin column volume 250cm
3, i.e. (1BV=250ml), absorption flow velocity 1～2BV/h, select polar macroporous resin for use: mean particle size is about 50 orders, and its effluent is theine and pigment, color from depth to shallow, absorption finishes; Clean with 2BV water, flow velocity 1BV/h is colourless to effluent; With 70% the ethanolic soln desorb of 2BV, flow velocity is collected coloured effluent (catechin solution) at 1BV/h;
4) membrane sepn with effluent at normal temperatures, pumps in the membrane separation plant, selects for use the polymer ceramic film to separate, and collecting liquid is EGCG solution;
5) crystallization, with EGCG solution at 50 ℃ of vacuum concentration, to solid content about 25%, and place crystallization under 5～10 ℃ of environment, crystallization use water rinse after accomplishing, must white EGCG crystal;
6) lyophilize of EGCG crystal is got white solid state EGCG product 2.13g, purity is 98.2%, and yield is 42.6%.
Embodiment 2:
1) extracts, oolong water liquid is carried out water carry and obtain tea liquid.
2) membrane filtration membrane-concentrated under the normal temperature, adopts the organic polymer rolled film to carry out removal of impurities and discolors, and TPS is removed in continuous extraction again, must purer tea-polyphenol appearance liquid (TP >=98%, EGCG >=50%).
3) chromatographic separation: with 120ml tea-polyphenol appearance liquid, its tea-polyphenol component is about 12g, at normal temperatures and pressures, the tea-polyphenol solution pump is gone in the resin adsorption column resin column volume 250cm
3, i.e. (1BV=250ml), absorption flow velocity 1～2BV/h, select polar macroporous resin for use: mean particle size is about 50 orders, and its effluent is theine and pigment, color from depth to shallow, absorption finishes; Clean with 2BV water, flow velocity 1BV/h is colourless to effluent; With 75% the ethanolic soln desorb of 2BV, flow velocity is collected coloured effluent (catechin solution) at 1BV/h;
4) membrane sepn with effluent at normal temperatures, pumps in the membrane separation plant, selects for use the polymer ceramic film to separate, and collecting liquid is EGCG solution;
5) crystallization, with EGCG solution at 60 ℃ of vacuum concentration, to solid content 30%, and place crystallization under 5～10 ℃ of environment, crystallization use water rinse after accomplishing, must white EGCG crystal;
6) lyophilize of EGCG crystal is got white solid state EGCG product 2.52g, purity is 98.2%, and yield is 42.0%.
Embodiment 3:
1) extracts, oolong water liquid is carried out water carry and obtain tea liquid.
2) membrane filtration membrane-concentrated under the normal temperature, adopts the organic polymer rolled film to carry out removal of impurities and discolors, and TPS is removed in continuous extraction again, must purer tea-polyphenol appearance liquid (TP >=98%, EGCG >=50%).
3) chromatographic separation: with 200ml tea-polyphenol appearance liquid, its tea-polyphenol component is about 20g, at normal temperatures and pressures, the tea-polyphenol solution pump is gone in the resin adsorption column resin column volume 250cm
3, i.e. (1BV=250ml), absorption flow velocity 1～2BV/h, select polar macroporous resin for use: mean particle size is about 50 orders, and its effluent is theine and pigment, color from depth to shallow, absorption finishes; Clean with 2BV water, flow velocity 1BV/h is colourless to effluent; With 80% the ethanolic soln desorb of 2BV, flow velocity is collected coloured effluent (catechin solution) at 1BV/h;
4) membrane sepn with effluent at normal temperatures, pumps in the membrane separation plant, selects for use the polymer ceramic film to separate, and collecting liquid is EGCG solution;
5) crystallization, with EGCG solution at 70 ℃ of vacuum concentration, to solid content 45%, and place crystallization under 5～10 ℃ of environment, crystallization use water rinse after accomplishing, must white EGCG crystal;
6) lyophilize of EGCG crystal is got white solid state EGCG product 4.31g, purity is 98.2%, and yield is 43.1%.
Claims (3)
1. method that adopts chromatography and membrane technique extracting epigallocatechin gallic acid ester from oolong tea is characterized in that may further comprise the steps:
(1) extract, with oolong through water carry tea liquid;
(2) membrane filtration membrane-concentrated under the normal temperature, adopts the organic polymer rolled film to carry out removal of impurities and discolors, and TPS is removed in continuous extraction again, must purer tea-polyphenol appearance liquid;
(3) chromatographic separation, selecting volume for use is 2500cm
3, height is 70～100cm pillar, inserts the polarity resin; Mean particle size is inserted pillar with appearance liquid again about 50 orders, utilize resin absorption catechin component, removes impurity such as theine, pigment, and flow velocity is 1～2BV/h; Effluent is shoaled by scarlet; The water that adds 1～2BV amount cleans, and flow velocity is constant, is colourless to effluent; Using 1～2BV, concentration is that 70～80% ethanolic soln carries out desorb, and flow velocity is constant, collects coloured effluent, and this effluent is a catechin solution;
(4) membrane sepn under the normal temperature, pumps into catechin solution in the membrane separation plant, adopts polymeric membrane to separate, and the collection liquid after the separation is EGCG solution;
(5) crystallization is carried out vacuum concentration with EGCG solution, and temperature is 50 ℃～70 ℃, the EGCG liquid concentrator is placed crystallization under 5～10 ℃ of environment after making its solid content be increased to 25-45%, wait crystallization fully after, rinsing gets the EGCG crystal;
(6) lyophilize gets white solid EGCG product with the lyophilize of EGCG crystal.
2. a kind of method that adopts chromatography and membrane technique extracting epigallocatechin gallic acid ester from oolong tea according to claim 1 is characterized in that the described polymeric membrane of above-mentioned steps (4) is a ceramic membrane, and the molecular weight that dams is 450～460.
3. a kind of method that adopts chromatography and membrane technique extracting epigallocatechin gallic acid ester from oolong tea according to claim 1; It is characterized in that described in the above-mentioned steps (5) EGCG solution being carried out vacuum concentration; Temperature is 60 ℃, and solid content is increased to 30%.
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| CN2010101782510A CN101921253B (en) | 2010-05-14 | 2010-05-14 | Method for extracting epigallocatechin gallic acid ester from oolong tea by chromatography and membrane technology |
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| CN2010101782510A CN101921253B (en) | 2010-05-14 | 2010-05-14 | Method for extracting epigallocatechin gallic acid ester from oolong tea by chromatography and membrane technology |
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| CN101921253B true CN101921253B (en) | 2012-05-09 |
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| CN102276571B (en) * | 2011-09-19 | 2013-06-19 | 湖南农业大学 | Method for preparing high-purity epigallocatechin |
| CN103819444B (en) * | 2014-02-26 | 2015-12-02 | 成都华高生物制品有限公司 | A kind of method extracting monomer EGCG from fresh tea leaf in its |
| CN104311522B (en) * | 2014-09-09 | 2016-08-24 | 湖南农业大学 | A kind of method that EGCG is prepared in separation from Folium Camelliae sinensis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1465572A (en) * | 2002-06-21 | 2004-01-07 | 浙江大学 | Method for purifying monomer of epigallocatechingallate (EGCG) |
| CN101381359A (en) * | 2008-10-15 | 2009-03-11 | 山东农业大学 | Method for extracting high-purity epigallocatechin-3-gallate from green tea |
| CN101555293A (en) * | 2009-05-05 | 2009-10-14 | 西藏奇正原生态健康品有限公司 | Method for extracting beta- glucosans from bran of corn |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1465572A (en) * | 2002-06-21 | 2004-01-07 | 浙江大学 | Method for purifying monomer of epigallocatechingallate (EGCG) |
| CN101381359A (en) * | 2008-10-15 | 2009-03-11 | 山东农业大学 | Method for extracting high-purity epigallocatechin-3-gallate from green tea |
| CN101555293A (en) * | 2009-05-05 | 2009-10-14 | 西藏奇正原生态健康品有限公司 | Method for extracting beta- glucosans from bran of corn |
Non-Patent Citations (3)
| Title |
|---|
| 尹军峰,权启爱,罗龙新,钱晓军.绿茶汁澄清工艺的膜分离技术研究.《茶叶科学》.2001,第21卷(第2期),116-119. * |
| 王瑞芳,陈发河,吴光斌,张凌晶.超滤法提纯茶多酚的研究.《膜科学与技术》.2009,第29卷(第4期),112-115. * |
| 高彦华.茶多酚提取及EGCG纯化新工艺研究.《中国优秀硕士学位论文全文数据库》.2006,全文. * |
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