CN1370766A - Green extraction process of high-purity tea polyphenol - Google Patents

Green extraction process of high-purity tea polyphenol Download PDF

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Publication number
CN1370766A
CN1370766A CN 01106878 CN01106878A CN1370766A CN 1370766 A CN1370766 A CN 1370766A CN 01106878 CN01106878 CN 01106878 CN 01106878 A CN01106878 A CN 01106878A CN 1370766 A CN1370766 A CN 1370766A
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China
Prior art keywords
tea
tea polyphenol
polyphenol
polymeric amide
catechin
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CN 01106878
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Chinese (zh)
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CN1147455C (en
Inventor
周春山
蒋新宇
钟世安
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Central South University
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Central South University
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Abstract

The pollution-free extraction process of high-purity tea polyphenol comprises treating tea extracting liquid through salting out process with polyamide as adsorbent, and acid aqueous solution of citric acid as washing agent to separate tea polyphenol from caffeine and pigment. The present invention has advantages of high tea polyphenol yield, improved product colour and luster and raised total content of catechin and its active component fat soluble catechin. Using no toxic organic solvent and heavy metal ions, the process is pollution frae. The said process had advantages of tea polyphenol extracting rate higher than 85%, tea polyphenol content in product higher than 99 % and total content of catechin as high as 80%.

Description

Green extraction process of high-purity tea polyphenol
The present invention relates to the extraction process of tea-polyphenol in a kind of tealeaves, belong to the natural organic chemistry field.
The extraction of tea-polyphenol is concluded by chemical process in the tealeaves at present, mainly can be divided into solvent extration and ion precipitation method two big classes.Two kinds of methods all are to be to extract solvent with water, and extracting solution directly must contain the filtrate of tea-polyphenol after filtration.When adopting solvent extration, to remove pigment and caffeine, raffinate is used the ethyl acetate extraction tea-polyphenol again with chloroform extraction filtrate; And ion precipitation rule Al 3+, Zn 2+, Fe 3+, Ca 2+Deng tea-polyphenol in the precipitation by metallic ion filtrate, it is separated with pigment and caffeine, the tea-polyphenol precipitation is used the ethyl acetate extraction tea-polyphenol again after acid is molten, and the ethyl acetate solution that contains tea-polyphenol at last is through precipitation, and vacuum-drying gets the tea-polyphenol product.Two kinds of methods can both obtain the tea-polyphenol of certain purity, but solvent extration has used deleterious chloroparaffin, ion precipitation rule heavy metal ion, the toxic residue that all may cause product, do not meet environmental requirement, in addition tea-polyphenol purity particularly wherein the content of active ingredient catechin also need further raising.
In order to overcome above-mentioned defective, it is simple to the invention provides a kind of technology, green non-pollution, and the extraction efficiency height, constant product quality can be produced high-purity tea polypenols and tea-polyphenol extraction process that wherein activeconstituents ester catechin content is high.
The present invention adopts the salt analysis method to handle tea extract, and the employing polymeric amide is a sorbent material, and acid aqueous citric acid solution is that washing composition makes tea-polyphenol separate with pigment with caffeine, and concrete processing condition are:
(1) lixiviate: dry tealeaves was pulverized the 0.5mm sieve, used flooding 1~1.5 hour, and 90~100 ℃ of water temperatures, solid-to-liquid ratio are W: V1=5~10;
(2) saltout: add sodium-chlor in the tealeaves vat liquor, control its concentration 3~5%, leave standstill and saltout 1 hour;
(3) polymeric amide absorption: vat liquor gained filtrate after routine is filtered is gone up the polymeric amide adsorption column, is 0.6~0.8mm with the polymeric amide particle diameter;
(4) washing: the aqueous citric acid solution washing polyamide column with pH is 2.5~4.0 removes caffeine and pigment;
(5) wash-out: tea-polyphenol desorb from the polyamide column is got off with the 60-85% ethanolic soln;
(6) ethyl acetate extraction: contain the tea-polyphenol ethanolic soln after ethanol is reclaimed in underpressure distillation, use the ethyl acetate extraction concentrated solution, the two-phase volume ratio is 1: 1;
(7) precipitation: the acetic acid ethyl acetate extract underpressure distillation removes most solvents and gets concentrated solution;
(8) vacuum-drying: concentrated solution vacuum-drying gets powder crystal attitude tea-polyphenol.
Among the present invention, tea extract is handled through saltouing can not only improve the tea-polyphenol extraction yield, improves its color and luster, and helps improving the content of catechin total amount and main active ingredient ester dissolubility catechin (as EGCG); Utilize polymeric amide absorption, the aqueous citric acid solution washing removes pigment and caffeine, has avoided the use of poisonous organic solvent and heavy metal ion, whole technological process green non-pollution.Adopt method of the present invention, the tea-polyphenol extraction yield is greater than 85%, and content is greater than 99%, and wherein the catechin total amount is up to 80%, and organic solvent-free and heavy metal ion are residual.
Embodiment:
1. green tea is produced through following processing step in the Hunan: and tealeaves pulverizings → boiling water lixiviate → 4-5% sodium-chlor saltouts → filters → and polyamide column absorption → pH3.0 aqueous citric acid solution washs → 80% aqueous ethanolic solution wash-out → concentrating under reduced pressure recovery ethyl acetate → enriched material vacuum-drying and gets powder crystal attitude tea-polyphenol.Tea-polyphenol extraction yield 88.5%, polyphenol content 99.4%, wherein the catechin total amount 80.2%, and EGCG content 50.4%, content of caffeine are pale yellow or white crystalline powdery less than 0.2%.

Claims (1)

1. green extraction process of high-purity tea polyphenol, it is characterized in that: the present invention adopts the salt analysis method to handle tea extract, the employing polymeric amide is a sorbent material, and acid aqueous citric acid solution is that washing composition makes tea-polyphenol separate with pigment with caffeine, and concrete processing condition are:
(1) saltouts: add sodium-chlor in the tealeaves vat liquor, control its concentration 3~5%, leave standstill and saltout 1 hour;
(2) polymeric amide absorption: vat liquor gained filtrate after routine is filtered is gone up the polymeric amide adsorption column, is 0.6~0.8mm with the polymeric amide particle diameter;
(3) washing: the aqueous citric acid solution washing polyamide column with pH is 2.5~4.0 removes caffeine and pigment.
CNB011068787A 2001-02-21 2001-02-21 Green extraction process of high-purity tea polyphenol Expired - Fee Related CN1147455C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB011068787A CN1147455C (en) 2001-02-21 2001-02-21 Green extraction process of high-purity tea polyphenol

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Application Number Priority Date Filing Date Title
CNB011068787A CN1147455C (en) 2001-02-21 2001-02-21 Green extraction process of high-purity tea polyphenol

Publications (2)

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CN1370766A true CN1370766A (en) 2002-09-25
CN1147455C CN1147455C (en) 2004-04-28

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CNB011068787A Expired - Fee Related CN1147455C (en) 2001-02-21 2001-02-21 Green extraction process of high-purity tea polyphenol

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100379732C (en) * 2006-02-28 2008-04-09 浙江大学 Method for removing caffeine from theapolyphenol coarse extract
CN100387587C (en) * 2005-12-29 2008-05-14 谢君 Process for separating purifying actived tea polyphenols
CN101120684B (en) * 2004-04-22 2011-03-30 中国海洋大学 Method for preparing biological preparation for decreasing organic phosphorous pesticide residue and promoting growth
CN103421051A (en) * 2013-08-02 2013-12-04 浙江大学 Method for preparing tea polyphenol by adsorption method
CN105566403A (en) * 2016-01-20 2016-05-11 黔南民族师范学院 Method for extracting high-purity tea polyphenols from Duyun tippy tea dust, tea tree branches and deposed tea

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101120684B (en) * 2004-04-22 2011-03-30 中国海洋大学 Method for preparing biological preparation for decreasing organic phosphorous pesticide residue and promoting growth
CN100387587C (en) * 2005-12-29 2008-05-14 谢君 Process for separating purifying actived tea polyphenols
CN100379732C (en) * 2006-02-28 2008-04-09 浙江大学 Method for removing caffeine from theapolyphenol coarse extract
CN103421051A (en) * 2013-08-02 2013-12-04 浙江大学 Method for preparing tea polyphenol by adsorption method
CN105566403A (en) * 2016-01-20 2016-05-11 黔南民族师范学院 Method for extracting high-purity tea polyphenols from Duyun tippy tea dust, tea tree branches and deposed tea

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Publication number Publication date
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