CN1097411A - A kind of production method of tea-polyphenol of caffein-free - Google Patents
A kind of production method of tea-polyphenol of caffein-free Download PDFInfo
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- CN1097411A CN1097411A CN 94105114 CN94105114A CN1097411A CN 1097411 A CN1097411 A CN 1097411A CN 94105114 CN94105114 CN 94105114 CN 94105114 A CN94105114 A CN 94105114A CN 1097411 A CN1097411 A CN 1097411A
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- polyphenol
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Abstract
From broken green tea, extract the production method of the tea-polyphenol of caffein-free, it is characterized in that using useful or harmless to health, water-soluble big ionizable metal salt precipitation tea-polyphenol, make its with millet paste in trimethyl-xanthine separate, the adsorbed a small amount of trimethyl-xanthine of tea-polyphenol salt is removed with gac, diatomite adsorbant again, and last extraction solvent still can be selected tea-polyphenol solubleness big except that ethyl acetate, this solubleness in water is little, simultaneously high, the not nontoxic organic solvent of boiling point.The invention provides a kind of Production Flow Chart safety, less investment, cost is low, extracts the high Preparing Tea-polyphenol technology of collection, is applicable to suitability for industrialized production.
Description
The invention belongs to tea Processing method, especially belong to the production method of from tealeaves, extracting the tea-polyphenol of caffein-free.This tea-polyphenol not only can be used as new food additive, and the antioxygen that is used for grease and oleaginous food and makeup is fresh-keeping, and pharmaceutically also is being the natural drug that a class utmost point has exploitation to be worth.It has the effect of very strong removing free radical, has multiple physiological actions such as suppressing cell mutation and canceration, anti-oxidant, step-down, radioprotective.
Extract high-content tea-polyphenol (more than 90%) at present both at home and abroad, following several class methods are roughly arranged: one, broken tea concentrates with water-containing organic solvent (methyl alcohol, ethanol, acetone etc.) lixiviate, with ether and ethyl acetate continuous extraction, evaporation drying etc.As day the disclosure specially permit clear 59-45385(1984), clear 61-13085(1986), CN 1034947A(1988).Two, make tea-polyphenol complex compound sediment in the millet paste with calcium hydroxide, separate with water layer, tea-polyphenol calcium changes molten back spraying drying with acid, or with ethyl acetate extraction, concentrating under reduced pressure, vacuum-drying.As CN 1043730A(1988), CN 1056679A(1990).Three, the lixiviate of broken tea boiling water, filtrate is adsorbed with polymer macroporous resin or gel, and organic solvent (methyl alcohol, ethanol or acetone etc.) wash-out concentrates and reclaims solvent, and the tea-polyphenol crude product is re-refined.As day the disclosure specially permit clear 65-311474(1990), clear 66-14572(1991), CN 1067359A(1991), CN1076926A(1992).
More than several class methods though characteristics are respectively arranged, its relative merits and limitation are arranged in application.Water-containing organic solvent extracts, its complex process, and required equipment is more, and energy consumption is big, contains trimethyl-xanthine in the product.Though calcium hydroxide precipitator method technology is simple,, can only say theoretical meaning because calcium hydroxide solubleness in water is very little.
The objective of the invention is to overcome the weak point that prior art exists, the production method of the tea-polyphenol of a kind of Production Flow Chart safety, cost is low, extraction yield is high caffein-free is provided, be applicable to suitability for industrialized production.
Content of the present invention is achieved through the following technical solutions:
With broken green tea is raw material, by the boiling water lixiviate, separate, purifying and drying and other steps, wherein: the boiling water vat liquor after filtering, add calcium chloride or complex-precipitation agent such as zinc chloride or zinc sulfate in the filtrate, add sig water after cooling, make PH reach 6.5～10, form tea-polyphenol calcium or tea-polyphenol zinc precipitation, filter, make that most of trimethyl-xanthine separates with precipitation in the millet paste, precipitate and use inorganic acid solution, handle with activated carbon-diatomite adsorbant again, refilter, remove residual trimethyl-xanthine, filtrate is with tea-polyphenol in the extraction solvent extraction water such as ethyl acetate, dry ester layer, reduction vaporization reclaims extraction solvent, and vacuum-drying promptly gets the tea-polyphenol finished product of caffein-free.
Calcium chloride or zinc chloride as the complex-precipitation agent in the above-mentioned steps can be used saturated solution, also can add solid calcium chloride or zinc chloride.
Alkali lye will be after solution cooling, and adds under stirring fast, avoids local alkalescence strong and cause the oxidation of tea-polyphenol calcium or tea-polyphenol zinc.
As dissolving tea-polyphenol calcium or the sedimentary mineral acid of tea-polyphenol zinc can be dilute hydrochloric acid or dilute sulphuric acid (Chinese Pharmacopoeia standard).
Sorbent material can be selected activated carbon (20-50 order)-diatomite for use, further removing the trimethyl-xanthine of being brought into by the absorption of tea-polyphenol calcium tea-polyphenol or zinc precipitation, does not influence when using when containing 1% trimethyl-xanthine in the tea-polyphenol, can save this step of absorption.
Extraction solvent also can be selected propyl acetate, isopropyl acetate, n-butyl acetate for use, isobutyl acetate, ethyl propionate, butyl formate, tetryl formates etc. are big to tea-polyphenol solubleness, and itself solubleness in water is little, simultaneously high, the not nontoxic again organic solvent of boiling point.
The inventive method has following advantage than prior art:
1, applying high density calcium ion (CaCl
2) or zine ion (ZnCl
2Or ZnSO
4), the consumption of water is significantly reduced, the consumption that helps improving the tea-polyphenol yield and reduce organic extractant reduces production costs.
2, very low with the caffeine content in the tea-polyphenol of present method production, (＜0.5%).
3, produce tea-polyphenol with present method, production cost is low, and industrial applicibility is strong, and Production Flow Chart safety.
The present invention will be further described in conjunction with attached embodiment.
Embodiment 1:
Get the 200 broken green tea of gram (or tea dust, tea powder) and add 8-10 times of boiling water, stir the extraction secondary, each 20-40 minute, press filtration merges the secondary vat liquor, adds the full solution 14ml(that closes of calcium chloride and contains calcium chloride 11 grams), cooling, stir (avoiding local alkalescence to cause the oxidation of tea-polyphenol calcium or tea-polyphenol zinc by force) fast and with 3N sodium hydroxide millet paste PH is transferred to 6.5-10 down, make tea-polyphenol calcium or tea-polyphenol zinc precipitation fully, tell precipitation (the recyclable caffeine of clear liquid) with whizzer.Put into dilute hydrochloric acid (Chinese Pharmacopoeia standard) in the precipitation, it is dissolved fully, add activated carbon (20-50 order), diatomite mixed adsorbent 2-4 restrains (weight ratio 1: 1), further remove the trimethyl-xanthine of bringing into by tea-polyphenol calcium or tea-polyphenol zinc co-precipitation absorption.Filtering separation, (ethyl acetate has/100 milliliters of suitable solubleness 9.7 grams to water in water with the propyl acetate extraction, 18 ℃), ester layer desiccant dehydration, the decompression rotary evaporation reclaims extraction solvent, finished product vacuum-drying, can get faint yellow coarse-grain attitude tea-polyphenol 12-16 gram, yield 6-8%, the Polyphenols total amount is more than 95%.
Embodiment 2:
Get 200 gram green tea ends and add 8-10 times of boiling water, stirring and leaching secondary, each 20 minutes, press filtration merges secondary raffinate, adds zinc chloride strong solution 13ml(and contains zinc chloride 13.5 grams), cooling is stirred fast down and with 10% ammonium hydroxide millet paste PH is transferred to 7-10, makes tea-polyphenol zinc precipitation fully.Below handle similar embodiment 1, but replace propyl acetate to make extraction tea-polyphenol solvent with ethyl acetate, tea-polyphenol yield 6-8%, the tea-leaf producing area difference, yield has height slightly.Polyphenol content (records by international tartrate iron colorimetry) more than 95%.
Replace zinc chloride to obtain similar results with zinc sulfate.
Manganous sulfate (Mn
Lv) and sal epsom (Mg
Lv) add dilute alkali with millet paste in complex compound solubleness in water of forming of tea-polyphenol bigger, be not suitable for and from tealeaves, extract tea-polyphenol.
Embodiment 3:
With methylene dichloride or chloroform extraction a small amount of trimethyl-xanthine that adsorbs in tea-polyphenol calcium or the tea-polyphenol zinc is removed tea-polyphenol zinc precipitation among tea-polyphenol calcium deposit among the embodiment 1 or the embodiment 2, filtered and tell methylene dichloride or chloroform.Tea-polyphenol calcium or tea-polyphenol zinc precipitation are with diluted hydrochloric acid dissolution, big with ethyl propionate or n-butyl acetate etc. to tea-polyphenol solubleness, this solubleness in water is little, high, the not nontoxic organic solvent extraction of while boiling point, drying and dehydrating, the decompression thin film evaporation reclaims organic solvent, and finished product vacuum-drying also can get the tea-polyphenol of caffein-free, and yield and product effective component content are the same.
Claims (4)
1, a kind of production method of tea-polyphenol of caffein-free, make raw material with broken green tea, by the boiling water lixiviate, separate, purifying and drying and other steps, it is characterized in that: the vat liquor filtrate filtered adds complex-precipitation agent calcium chloride or zinc chloride, add sig water after cooling, make PH reach 6.5～10, form tea-polyphenol calcium or tea-polyphenol zinc precipitation, filter, the precipitation inorganic acid solution, handle with activated carbon-diatomite adsorbant, filter, filtrate extracts with extraction solvents such as ethyl acetate, dry ester layer, reduction vaporization reclaims extraction solvent, and vacuum-drying promptly gets the tea-polyphenol finished product of caffein-free.
2, method according to claim 1, it is characterized in that dissolving tea-polyphenol calcium or the sedimentary mineral acid of tea-polyphenol zinc can be dilute hydrochloric acid or dilute sulphuric acid (Chinese Pharmacopoeia standard).
3, method according to claim 1 is characterized in that sorbent material can select activated carbon (20-50 order) diatomite for use, removing residual trimethyl-xanthine, or does not influence when using when containing 1% trimethyl-xanthine in the tea-polyphenol, can save this step of absorption.
4, method according to claim 1, it is characterized in that extraction solvent also can select for use propyl acetate, isopropyl acetate, n-butyl acetate, isobutyl acetate, ethyl propionate, butyl formate, tetryl formate etc. big to tea-polyphenol solubleness, this solubleness in water is little, simultaneously high, the not nontoxic organic solvent of boiling point.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94105114 CN1097411A (en) | 1994-05-19 | 1994-05-19 | A kind of production method of tea-polyphenol of caffein-free |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94105114 CN1097411A (en) | 1994-05-19 | 1994-05-19 | A kind of production method of tea-polyphenol of caffein-free |
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| Publication Number | Publication Date |
|---|---|
| CN1097411A true CN1097411A (en) | 1995-01-18 |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996028178A1 (en) * | 1995-03-14 | 1996-09-19 | Indena S.P.A. | Polyphenol fractions of tea, the use thereof and formulations containing them |
| CN100404523C (en) * | 2006-02-21 | 2008-07-23 | 张守政 | Process for extracting tea polyphenol, theanine, tea polysaccharide and tea pigment from tea |
| CN102225122A (en) * | 2011-06-09 | 2011-10-26 | 四川中测科技投资有限公司 | Caffeine-free tea polyphenol and preparation method thereof |
| CN102503964A (en) * | 2011-11-11 | 2012-06-20 | 河南大学 | Preparation process for tea polyphenol metal complex |
| CN102603498A (en) * | 2012-02-08 | 2012-07-25 | 厦门大学 | Method for extracting phenolic compounds from biological oil |
| CN102771614A (en) * | 2012-08-10 | 2012-11-14 | 福建农林大学 | Processing technology of black tea with low caffeine |
| CN104286911A (en) * | 2014-10-02 | 2015-01-21 | 滕元妹 | Preparation method of Miao health-preservation oil-sealed salted meat |
| CN105503967A (en) * | 2016-01-04 | 2016-04-20 | 广州孺子牛生物科技有限公司 | Method for directly synthesizing tea polyphenol metal complex with tea as raw material |
| CN108516995A (en) * | 2018-04-27 | 2018-09-11 | 湖南口味王集团有限责任公司 | A kind of method of purification of betel nut polyphenol |
| CN108706675A (en) * | 2018-05-31 | 2018-10-26 | 华南理工大学 | A method of it substituting DIPE and coal chemical industrial waste water containing phenol is extracted |
| CN110354816A (en) * | 2019-05-31 | 2019-10-22 | 中国农业科学院茶叶研究所 | A kind of chitosan/oxidized graphene/silicon diatomaceous earth composite material and preparation method, application |
| CN115868559A (en) * | 2022-12-14 | 2023-03-31 | 湖北神武绿源农业科技有限公司 | Preparation method of instant green tea powder |
-
1994
- 1994-05-19 CN CN 94105114 patent/CN1097411A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5989557A (en) * | 1995-03-14 | 1999-11-23 | Indena S.P.A. | Process for extracting polyphenol fractions of tea and compositions produced therewith |
| US6096359A (en) * | 1995-03-14 | 2000-08-01 | Indena S.P.A. | Polyphenol fractions of tea, the use thereof and formulations containing them |
| WO1996028178A1 (en) * | 1995-03-14 | 1996-09-19 | Indena S.P.A. | Polyphenol fractions of tea, the use thereof and formulations containing them |
| CN100404523C (en) * | 2006-02-21 | 2008-07-23 | 张守政 | Process for extracting tea polyphenol, theanine, tea polysaccharide and tea pigment from tea |
| CN102225122A (en) * | 2011-06-09 | 2011-10-26 | 四川中测科技投资有限公司 | Caffeine-free tea polyphenol and preparation method thereof |
| CN102503964B (en) * | 2011-11-11 | 2015-04-22 | 河南大学 | Preparation process for tea polyphenol metal complex |
| CN102503964A (en) * | 2011-11-11 | 2012-06-20 | 河南大学 | Preparation process for tea polyphenol metal complex |
| CN102603498A (en) * | 2012-02-08 | 2012-07-25 | 厦门大学 | Method for extracting phenolic compounds from biological oil |
| CN102771614A (en) * | 2012-08-10 | 2012-11-14 | 福建农林大学 | Processing technology of black tea with low caffeine |
| CN104286911A (en) * | 2014-10-02 | 2015-01-21 | 滕元妹 | Preparation method of Miao health-preservation oil-sealed salted meat |
| CN105503967A (en) * | 2016-01-04 | 2016-04-20 | 广州孺子牛生物科技有限公司 | Method for directly synthesizing tea polyphenol metal complex with tea as raw material |
| CN108516995A (en) * | 2018-04-27 | 2018-09-11 | 湖南口味王集团有限责任公司 | A kind of method of purification of betel nut polyphenol |
| CN108706675A (en) * | 2018-05-31 | 2018-10-26 | 华南理工大学 | A method of it substituting DIPE and coal chemical industrial waste water containing phenol is extracted |
| CN110354816A (en) * | 2019-05-31 | 2019-10-22 | 中国农业科学院茶叶研究所 | A kind of chitosan/oxidized graphene/silicon diatomaceous earth composite material and preparation method, application |
| CN110354816B (en) * | 2019-05-31 | 2022-05-27 | 中国农业科学院茶叶研究所 | Chitosan/graphene oxide/diatomite composite material and preparation method and application thereof |
| CN115868559A (en) * | 2022-12-14 | 2023-03-31 | 湖北神武绿源农业科技有限公司 | Preparation method of instant green tea powder |
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