CN101703130B - Technology for producing green tea extract - Google Patents
Technology for producing green tea extract Download PDFInfo
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- CN101703130B CN101703130B CN2009101543926A CN200910154392A CN101703130B CN 101703130 B CN101703130 B CN 101703130B CN 2009101543926 A CN2009101543926 A CN 2009101543926A CN 200910154392 A CN200910154392 A CN 200910154392A CN 101703130 B CN101703130 B CN 101703130B
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Abstract
The invention relates to a technology for producing green tea extract, belonging to the technical field of plant extraction and comprising the following steps: adding green tea raw material into eight times of 50-70% of ethanol, dividing green tea leaves into three portions to extract under the temperature of 70 DEG C, collecting extracting solution, evaporating in vacuum, recovering the ethanol, centrifuging and collecting supernatant; and leading the centrifuged extracting solution to pass through a macroporous resin chromatographic column with the ratio of diameter to height being 1:10, rinsing in batches by 5-15% of ethanol, desorbing by using 70% of ethanol, collecting stripping liquid after desorbing, leading the stripping liquid to pass through a macroporous resin chromatographic column with the ratio of diameter to height being 1:30, collecting the stripping liquid, recovering ethanol by reduced pressure, concentrating into thick paste, and drying in vacuum to obtain the green tea extract. The invention uses multiple extraction and multi-level decentralization, and adopts two methods of crude extraction and refined extraction to greatly improve the content of effective components; by the invention, epigallocatechin gallate (EGCG) monomer with a high content can be obtained.
Description
Technical field
The present invention relates to a kind of production technology of green-tea extract, belong to technical field of plant extraction.
Background technology
At present; Green-tea extract more and more receives people's favor because it has the effect than strong anti-oxidation property and prophylaxis of cancer and cardiovascular disease, at present; The active ingredient of extracting from green tea is mainly Tea Polyphenols; Be main with catechin especially again wherein, like L-Epicatechin gallate (ECG), epigallocatechin (EGC), Epigallo-catechin gallate (EGCG) (EGCG) and epicatechin compositions such as (EC), and especially the medical value of Epigallo-catechin gallate (EGCG) (EGCG) is more and more approved by people; At present, the method for distilling that is used for green tea mainly contains following several kinds: 1, the extraction-precipitation method; 2, solvent extraction method; 3, counter-current extraction+purifying precipitation method etc. adopts said method to extract the active ingredient of green tea, all has a shortcoming; At present owing to receive the influence of weather and acquisition time, green tea is of low quality at present exactly, and the active constituent content of the raw green tea leaf that is used to extract is more and more lower; And; In this case, adopt traditional production process, Epigallo-catechin gallate (EGCG) (EGCG) monomer is extracted with other active ingredients together; Its content is not high, causes often being difficult to obtain especially Epigallo-catechin gallate (EGCG) (EGCG) monomer.
Summary of the invention
To the problems referred to above of prior art, the object of the present invention is to provide a kind of production technology that can effectively improve green-tea extract content and purity.
The technical scheme that the present invention adopts is following, and a kind of production technology of green-tea extract is characterized in that, may further comprise the steps:
(1), extract green tea active ingredient: the ethanol that the green tea raw material is added 8 times 50～70% divides green tea and carries out lixiviate 3 times, and extraction temperature 70 degree are collected extract then, and ethanol is reclaimed in vacuum evaporation, extract through three grades centrifugal after the collection supernatant;
(2), upper prop desorb: it is 1: 10 macroreticular resin chromatographic column that the extract that will pass through centrifugal treating is crossed blade diameter length ratio; Ethanol with 5～15% drip washing to eluate in batches is clear and bright, uses 70% alcohol desorption then, after desorb finishes; Collect stripping liquid, decompression recycling ethanol; Is 1: 30 macroreticular resin chromatographic column with above-mentioned stripping liquid after blade diameter length ratio, uses 30%, 50%, 70% ethanol drip washing respectively successively three times, collects stripping liquid respectively, decompression recycling ethanol, be condensed into thick paste after, vacuum drying promptly gets green-tea extract.
Of the present invention further the setting as follows:
The green tea raw material comprises tealeaves, tea dust, tea ash.
3 lixiviates were respectively 3 hours for the first time, and 2.5 hours for the second time, 2 hours for the third time.
Said three grades centrifugal be carry out under 1000 commentaries on classics/min, 4400 commentaries on classics/min, the 14000 commentaries on classics/min centrifugal.
Need clean in advance to guarantee that cleaning is resin regeneration before crossing for the first time post, adopt alkali cleaning earlier, the back with the purified water flushing to neutral, then with pickling to pH value～4, again with the purified water flushing to neutral.
When for the first time crossing post, clear and bright to flowing out liquid after extract has been crossed with purified water drip washing, to remove the macromolecular substances in the macroreticular resin chromatographic column.
The blade diameter length ratio that adopts when crossing post for the second time is 1: 30 a macroreticular resin chromatographic column, for the aperture is 500mm, highly is the macroreticular resin chromatographic column of 15m.
Described blade diameter length ratio is 1: 30 a macroreticular resin chromatographic column, and the ethanol with 95% concentration before using cleans, and realizes resin regeneration.
Beneficial effect of the present invention is following:
1, adopt extracted many times, multistage centrifugal can be effectively complete with the extracts active ingredients of green tea raw material, and multistage centrifugal can be removed solid impurity in the extract and water-fast particulate matter simultaneously, for ready before the extract upper prop.
2, adopt and slightly to carry and essence is carried desorption method twice, the active ingredient desorb that helps extract is complete, and active constituent content is improved greatly;
3, adopting blade diameter length ratio is that 1: 30 macroreticular resin chromatographic column carries out essence and carries, and adopts competitive Adsorption and multistage to collect, and has improved the content of Epigallo-catechin gallate (EGCG) (EGCG) monomer greatly, makes product quality and is worth raising.
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is described further.
Description of drawings
Fig. 1 is a process chart of the present invention;
Fig. 2 is the structural representation of modified chromatographic column of the present invention.
The specific embodiment
In conjunction with shown in Figure 1, the production technology of green-tea extract of the present invention may further comprise the steps:
1, extracts green tea active ingredient
1.1, lixiviate: with green tea, tea dust, the tea ash collected, the ethanol that adds then 8 times 50～70% divides green tea and carries out lixiviate 3 times, and 3 hours for the first time, 2.5 hours for the second time, 2 hours for the third time, extraction temperature 70 degree were collected extract then.
1.2, ethanol reclaims: the vacuum evaporation extract, reclaim ethanol, it is subsequent use that extract adds water-cooled.
1.3, centrifugal: with extract through three grades centrifugal, respectively 1000 commentariess on classics/min, 4400 commentariess on classics/min, 14000 commentaries on classics/min, the centrifugal supernatant of collection afterwards.Wherein, First-stage centrifugal mainly is the large granular impurity of removing in the extract, and secondary is centrifugal mainly to be the granule impurity of removing in the extract, and three grades centrifugal mainly is the molecule impurity of removing in the extract; Centrifugal through three grades; Can effectively remove solid impurity and water-fast particulate matter in the concentrate, prevent behind the concentrate upper prop chromatographic column to be polluted, be difficult to regeneration.
2, upper prop desorb
2.1, for the first time cross post
It is 1: 10 macroreticular resin chromatographic column that the extract that will pass through centrifugal treating is crossed blade diameter length ratio, and the macroreticular resin chromatographic column need clean to guarantee that cleaning is resin regeneration in advance, adopts alkali cleaning earlier; The back, with pickling to pH value～4, is used to neutral with the purified water flushing then again; Purified water flushing is to neutral, and after extract had been crossed, crossing post with purified water, to be washed till outflow liquid clear and bright; Remove the macromolecular substances in the macroreticular resin chromatographic column, use 5～15% ethanol like 5%, 10%, 15% ethanol then, drip washing to eluate is clear and bright in batches; Removing in the macroreticular resin chromatographic column, the incompatible material of molecular weight and macroreticular resin aperture is used the active ingredient in 70% the alcohol desorption macroreticular resin chromatographic column then; After desorb finishes, collect stripping liquid, decompression recycling ethanol.
2.2, for the second time cross post
To pass through the stripping liquid of crossing for the first time post, to cross blade diameter length ratio be 1: 30 macroreticular resin chromatographic column, and blade diameter length ratio is 1: 30 a macroreticular resin chromatographic column, and promptly the aperture is 500mm; Highly be the macroreticular resin chromatographic column of 15m, the macroreticular resin chromatographic column need clean to guarantee to clean in advance promptly regenerates setting-out; After having crossed, cross post with purified water and be washed till that to flow out liquid clear and bright, three times (30% once to use 30%, 50%, 70% ethanol drip washing then respectively successively; 50% once, and 70% once), collect stripping liquid respectively; Decompression recycling ethanol, be condensed into thick paste after, vacuum drying promptly gets green-tea extract.The macroreticular resin chromatographic column, because extract is after for the first time crossing post, very clean (not having too much impurity) therefore with the ethanol cleaning of 95% concentration, can be realized resin regeneration.Stripping liquid after crossing post for the second time, the target product active constituent content is seen shown in the table 1.
It is 1: 30 macroreticular resin chromatographic column that the present invention has adopted blade diameter length ratio shown in Figure 2 with innovating, and takes the technology of twice upper prop, mainly utilizes the principle of adsorption chromatography and Partition Chromatography:
At first, the selectivity of target product (catechin, polyphenol) in the macroreticular resin chromatographic column is greater than other compositions, at upper prop process leading portion; Because polymeric adsorbent has than large space, at this moment, the target product in the extract and other compositions can both occupy-places in resin; And along with the increase of applied sample amount; The potential energy power of robbing of the target product in the extract is stronger, can progressively drive other compositions away and occupy-place, makes that abundance zone progressively amplifies on the chromatographic column; Thereby active ingredient ratio in extract is increased, improve content of effective in the green tea.
Secondly, owing to increased the blade diameter length ratio of chromatographic column, so just increased the enriched layer of the target product in the chromatographic column greatly; The content of target product is greatly enhanced; On the other hand, elongated in the extract target product and other compositions in the path of chromatographic column, and because the target product in the extract is different with the translational speed of other compositions on chromatographic column; Like this; Target product in the extract is widened with the distance of other compositions on chromatographic column, thereby realized the purpose of Fractional Collections, target product purity and content are greatly enhanced.
Therefore, the present invention carries through adopting slightly, essence is carried twice and crossed the processing step of post, and adopts the chromatographic column of big blade diameter length ratio, has following outstanding effect:
1, effectively improved content of effective in the extract, extract active constituent content catechin reaches as high as 98%, polyphenol about 78%.Specifically as shown in table 1.
2, can realize the multistage collection; The purity of extract is improved greatly; Improve greatly like Epigallo-catechin gallate (EGCG) (EGCG) content of monomer, solved traditional handicraft and can't obtain the especially difficult problem of Epigallo-catechin gallate (EGCG) (EGCG) monomer.
3, the present invention is through optimizing extraction, desorption technique; Even under the lower situation of raw materials quality, still can obtain the active constituent content high product, like this; Production cost is reduced, can obtain good use like the tea dust that originally not have utilization, tea ash etc.
Claims (5)
1. the production technology of a green-tea extract is characterized in that, may further comprise the steps:
(1), extract green tea active ingredient: the ethanol that the green tea raw material is added 8 times 50～70% divides green tea and carries out lixiviate 3 times, and extraction temperature 70 degree are collected extract then, and ethanol is reclaimed in vacuum evaporation, extract through three grades centrifugal after the collection supernatant; Described 3 lixiviates were respectively 3 hours for the first time, and 2.5 hours for the second time, 2 hours for the third time; Said three grades centrifugal be carry out under 1000 commentaries on classics/min, 4400 commentaries on classics/min, the 14000 commentaries on classics/min centrifugal;
(2), upper prop desorb: it is 1: 10 macroreticular resin chromatographic column that the extract that will pass through centrifugal treating is crossed blade diameter length ratio; Ethanol with 5～15% drip washing to eluate in batches is clear and bright, uses 70% alcohol desorption then, after desorb finishes; Collect stripping liquid, decompression recycling ethanol; Is 1: 30 macroreticular resin chromatographic column with above-mentioned stripping liquid after blade diameter length ratio, uses 30%, 50%, 70% ethanol drip washing respectively successively three times, collects stripping liquid respectively, decompression recycling ethanol, be condensed into thick paste after, vacuum drying promptly gets green-tea extract;
In the step 2: need clean in advance to guarantee that cleaning is resin regeneration before crossing for the first time post, adopt alkali cleaning earlier, the back with the purified water flushing to neutral, then with pickling to pH value～4, again with the purified water flushing to neutral;
2. the production technology of a kind of green-tea extract as claimed in claim 1 is characterized in that: clear and bright to flowing out liquid after extract has been crossed when crossing post for the first time with purified water drip washing, and to remove the macromolecular substances in the macroreticular resin chromatographic column.
3. the production technology of a kind of green-tea extract as claimed in claim 1 is characterized in that: the blade diameter length ratio that adopts when crossing post for the second time is 1: 30 a macroreticular resin chromatographic column, for the aperture is 500mm, highly is the macroreticular resin chromatographic column of 15m.
4. the production technology of a kind of green-tea extract as claimed in claim 3, it is characterized in that: described blade diameter length ratio is 1: 30 a macroreticular resin chromatographic column, the ethanol with 95% concentration before using cleans, the realization resin regeneration.
5. the production technology of a kind of green-tea extract as claimed in claim 1, it is characterized in that: said green tea raw material comprises tealeaves, tea dust.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101543926A CN101703130B (en) | 2009-12-03 | 2009-12-03 | Technology for producing green tea extract |
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| CN2009101543926A CN101703130B (en) | 2009-12-03 | 2009-12-03 | Technology for producing green tea extract |
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| CN101703130B true CN101703130B (en) | 2012-05-02 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104171150A (en) * | 2014-07-21 | 2014-12-03 | 云南农业大学 | Tea cream retaining original tea aroma and taste and processing technology thereof |
| CN105767326A (en) * | 2014-09-10 | 2016-07-20 | 邹玉华 | Green tea extract and preparation method thereof |
| CN105707973A (en) * | 2014-09-10 | 2016-06-29 | 邹玉华 | Green tea extract and preparation method thereof |
| CN104171157B (en) * | 2014-09-10 | 2016-06-15 | 河源市绿环生物科技有限公司 | A kind of green tea extract and preparation method thereof, application |
| CN106106921A (en) * | 2016-06-24 | 2016-11-16 | 四川省金桑庄园农业发展股份有限公司 | A kind of winter Mulberry herbal tea and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1286252A (en) * | 1999-08-16 | 2001-03-07 | 弗·哈夫曼-拉罗切有限公司 | Process for preparing epigallocatechin gallate |
| CN1733753A (en) * | 2005-08-12 | 2006-02-15 | 上海诺德生物实业有限公司 | Epigallocatechin gallate monomer purification method |
| CN101040713A (en) * | 2007-04-27 | 2007-09-26 | 乔泓程 | Health-care food having functions of oxidation resisting and immunity improving |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1286252A (en) * | 1999-08-16 | 2001-03-07 | 弗·哈夫曼-拉罗切有限公司 | Process for preparing epigallocatechin gallate |
| CN1733753A (en) * | 2005-08-12 | 2006-02-15 | 上海诺德生物实业有限公司 | Epigallocatechin gallate monomer purification method |
| CN101040713A (en) * | 2007-04-27 | 2007-09-26 | 乔泓程 | Health-care food having functions of oxidation resisting and immunity improving |
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