CN102225122B - Caffeine-free tea polyphenol and preparation method thereof - Google Patents
Caffeine-free tea polyphenol and preparation method thereof Download PDFInfo
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- CN102225122B CN102225122B CN2011101534661A CN201110153466A CN102225122B CN 102225122 B CN102225122 B CN 102225122B CN 2011101534661 A CN2011101534661 A CN 2011101534661A CN 201110153466 A CN201110153466 A CN 201110153466A CN 102225122 B CN102225122 B CN 102225122B
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Abstract
The invention relates to caffeine-free tea polyphenol and a preparation method thereof, and belongs to the field of separation and extraction. The invention solves a technical problem by providing a preparation method of caffeine-free tea polyphenol. The preparation method of caffeine-free tea polyphenol of the invention comprises the following steps: a. at least one of tea polyphenol containing caffeine and a tea extractive containing caffeine is condensed or dissolved with water and filtered, and an obtained filtrate is kept for use; b. the filtrate obtained in step a is sampled on a gel chromatographic column, washed out with 5-25wt% ethanol solution until 1.3-1.7 BV of eluent flows out, then washed out with 50-70tw% ethanol solution until 1.8-2.5BV of eluent flows out; the eluent of the 50-70tw% ethanol solution is collected, condensed and dried to obtain tea polyphenol. Filling material of the gel filtration chromatography is sephadex LH-20 or cross-link dextran agarose gel.
Description
Technical field
The present invention relates to not have theine tea-polyphenol and preparation method thereof, belong to the separation and Extraction field.
Background technology
Tea-polyphenol is the important activeconstituents of tea Ye Zhongyi class; Content is generally accounting for 18%～36% of dry weight of tea leaves, is a kind of natural inhibitor, can be widely used in industries such as food, medicine, healthcare products and makeup; Also possesses reducing blood-fat and blood sugar simultaneously; Hypotensive and SUV, arteriosclerosis, mutation and anticancer change, function such as anti-ageing, anti-oxidant, and be used for the multiple disease of clinical treatment.
At present, the method for preparing tea-polyphenol mainly contains solvent extration, resin absorption partition method and supercritical extraction.Solvent extration is that tea-polyphenol is produced the technology that the most generally adopts at present, and its yield is high, and cost is low, but quality product is lower, and content of caffeine is high, and organic solvent residual is high, and Environmental costs are high.But resin adsorption method production purity high product can reduce simultaneously organic solvent and use, but has the shortcoming that yield is lower, cost is high, the cycle is long, and can not effectively remove coffee thereby influence the quality of tea-polyphenol.Supercritical extraction with an organic solvent also can not get the low-caffeine tea-polyphenol, but product impurity is many, product purity is not high, and equipment input and maintenance cost are too high, operational condition is strict, realize that suitability for industrialized production also has certain difficulty.
Tea-polyphenol purity height, particularly theine and catechin content have directly determined the quality and the purposes of product.Therefore, no theine of preparation and the high tea-polyphenol of catechin content become the technical barrier that this area presses for solution at present.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method for preparing no theine tea-polyphenol.
The method that the present invention prepares no theine tea-polyphenol comprises the steps:
A, raw material prepare: contain theine tea-polyphenol, contain at least a in the tea leaf extract of theine, (, then concentrate through concentrating or being dissolved in water if raw material is a solution; If raw material is solid or semisolid; Then be dissolved in water,, preferably prepare the solution of high density for the ease of chromatographic separation; To satisfy the isolating needs of gel chromatography) after-filtration (being preferably membrane filtration), the gained filtrate for later use;
B, gel chromatography separate: a step gained filtrating is gone up appearance to gel chromatography column; Ethanolic soln with 5～25wt% is eluted to outflow 1.3～1.7BV elutriant; It is 1.8～2.5BV that the ethanolic soln of using 50～70wt% then instead continues to be eluted to effusive elutriant, collects the elutriant of the ethanolic soln of 50～70wt%, concentrates the elutriant of collecting; Dry (preferred vacuum lyophilization) obtains tea-polyphenol; Wherein, the used filler of said gel permeation chromatography is sephadex lh-20 or sephadex sepharose.
Wherein, the tea-polyphenol that contains theine in the above-mentioned a step, the tea leaf extract that contains theine can adopt the commercially available prod, also can prepare voluntarily.As the tea leaf extract that contains theine can adopt following method to be prepared from: adopt water or ethanolic soln lixiviate tealeaves, filter then, concentrate, obtain containing the tea leaf extract of theine.
Wherein, When water or ethanolic soln lixiviate tealeaves, the consumption of water or ethanolic soln is that conventional amount used gets final product, further; The consumption of water or ethanolic soln is preferably 6～70 times of tealeaves weight, and the consumption of water or ethanolic soln most preferably is 15～30 times of tealeaves weight.
Wherein, the ethanolic soln of concentration comprises that straight alcohol solution (being the above ethanolic soln of 95wt%) may be used to the lixiviate of tealeaves arbitrarily, and in order to reduce cost, the concentration of ethanolic soln is preferably 0～40wt% described in the above-mentioned a step.
Wherein,, in order to make not residual any organic reagent in the product, and reduce cost, preferably adopt water (boiling water) lixiviate tealeaves because water (boiling water) lixiviate tealeaves does not have notable difference with comparing with tea-polyphenol in the ethanolic soln lixiviate tealeaves.
Wherein, when preparation contains the tea leaf extract of theine, can adopt ordinary method to concentrate, concentrating means is preferably vacuum rotary steam and concentrates.
Further, in order to improve the quality of product, the flow velocity of above-mentioned b step during with the ethanolic soln wash-out of 5～25wt% is preferably 0.5～1.0BV/h, and the flow velocity of b step during with the ethanolic soln wash-out of 50～70wt% is preferably 0.5～1.0BV/h.
Further, in order to improve the quality of product, the b step of the inventive method most preferably is: gel chromatography separates: a step gained filtrating is gone up appearance to gel chromatography column; Be eluted to the flow velocity of 0.8BV/h with the ethanolic soln of 20wt% and flow out the 1.5BV elutriant; The ethanolic soln that uses 65wt% then continues to be eluted to effusive elutriant with the flow velocity of 0.8BV/h and is 2BV, collects the elutriant of 1.5～2BV, concentrates and collects liquid; Drying obtains tea-polyphenol.
Wherein, the used filler of the said gel permeation chromatography of above-mentioned b step is preferably sephadex lh-20.
The present invention also provides by the prepared no theine tea-polyphenol of aforesaid method.
The inventive method is simple to operate, and production efficiency is high, economic environmental protection, and it is residual that product does not have toxic reagent, and it is reliable to be used for industrial securities such as food, medicine.The inventive method gained tea-polyphenol purity can reach more than 98%, and is decaffeinated, is rich in catechin (catechin content can reach more than 90%), and wherein the strongest EGCG content of anti-oxidant activity is more than 60%.The present invention provides a kind of new selection for tea-polyphenol production high-quality, high added value, has broad application prospects
Description of drawings
Fig. 1 prepares the color atlas of tea-polyphenol for column chromatography for separation, and wherein, peak A is a tea-polyphenol;
Fig. 2 is the high-efficient liquid phase analysis color atlas, and among the figure, figure (A) is the color atlas of product; Figure (B) is the color atlas of tea leaf extract, and figure (C) is the color atlas of tealeaves biochemical component standard substance.
Embodiment
The method that the present invention prepares no theine tea-polyphenol comprises the steps:
A, raw material prepare: contain theine tea-polyphenol, contain at least a in the tea leaf extract of theine, (, then concentrate through concentrating or being dissolved in water if raw material is a solution; If raw material is solid or semisolid; Then be dissolved in water,, preferably prepare the solution of high density for the ease of chromatographic separation; To satisfy the isolating needs of gel chromatography) after-filtration (being preferably membrane filtration), the gained filtrate for later use;
B, gel chromatography separate: a step gained filtrating is gone up appearance to gel chromatography column; Ethanolic soln with 5～25wt% is eluted to outflow 1.3～1.7BV elutriant; It is 1.8～2.5BV that the ethanolic soln of using 50～70wt% then instead continues to be eluted to effusive elutriant, collects the elutriant of the ethanolic soln of 50～70wt%, concentrates the elutriant of collecting; Dry (preferred vacuum lyophilization) obtains tea-polyphenol; Wherein, the used filler of said gel permeation chromatography is sephadex lh-20 or sephadex sepharose.
Wherein, the tea-polyphenol that contains theine in the above-mentioned a step, the tea leaf extract that contains theine can adopt the commercially available prod, also can prepare voluntarily.As the tea leaf extract that contains theine can adopt following method to be prepared from: adopt water or ethanolic soln lixiviate tealeaves, filter then, concentrate, obtain containing the tea leaf extract of theine.
Wherein, When water or ethanolic soln lixiviate tealeaves, the consumption of water or ethanolic soln is that conventional amount used gets final product, further; The consumption of water or ethanolic soln is preferably 6～70 times of tealeaves weight, and the consumption of water or ethanolic soln most preferably is 15～30 times of tealeaves weight.
Wherein, the ethanolic soln of concentration comprises that straight alcohol solution (being the above ethanolic soln of 95wt%) may be used to the lixiviate of tealeaves arbitrarily, and in order to reduce cost, the concentration of ethanolic soln is preferably 0～40wt% described in the above-mentioned a step.
Wherein,, in order to make not residual any organic reagent in the product, and reduce cost, preferably adopt water (boiling water) lixiviate tealeaves because water (boiling water) lixiviate tealeaves does not have notable difference with comparing with tea-polyphenol in the ethanolic soln lixiviate tealeaves.
Wherein, when preparation contains the tea leaf extract of theine, can adopt ordinary method to concentrate, concentrating means is preferably vacuum rotary steam and concentrates.
Further, in order to improve the quality of product, the flow velocity of above-mentioned b step during with the ethanolic soln wash-out of 5～25wt% is preferably 0.5～1.0BV/h, and the flow velocity of b step during with the ethanolic soln wash-out of 50～70wt% is preferably 0.5～1.0BV/h.
Further, in order to improve the quality of product, the b step of the inventive method most preferably is: gel chromatography separates: a step gained filtrating is gone up appearance to gel chromatography column; Be eluted to the flow velocity of 0.8BV/h with the ethanolic soln of 20wt% and flow out the 1.5BV elutriant; The ethanolic soln that uses 65wt% then continues to be eluted to effusive elutriant with the flow velocity of 0.8BV/h and is 2BV, collects the elutriant of 1.5～2BV, concentrates and collects liquid; Drying obtains tea-polyphenol.
Wherein, the used filler of the said gel permeation chromatography of above-mentioned b step is preferably sephadex lh-20.
The present invention also provides by the prepared no theine tea-polyphenol of aforesaid method.
Do further description below in conjunction with the embodiment specific embodiments of the invention, therefore do not limit the present invention among the described scope of embodiments.
Embodiment 1 adopts the inventive method from tealeaves, to extract no theine tea-polyphenol
3g tealeaves adds boiling water 50ml lixiviate 30min; Cross the filter membrane in 0.45 μ m aperture; Filtrating concentrate to be gone up appearance to populated sephadex lh-20 (purchasing to GE medical treatment group) pillar, is eluted to outflow 1.5BV elutriant with the ethanolic soln of 20wt% with the flow velocity of 0.8BV/h then, uses the flow velocity continuation wash-out of the ethanolic soln of 65wt% with 0.8BV/h then instead; Collect the elutriant of 1.5～2BV, elutriant concentrates, vacuum lyophilization obtains product.
It is as shown in Figure 1 that column chromatography for separation prepares the color atlas of tea-polyphenol, and wherein, peak A is tea-polyphenol.According to standard " tea-polyphenol and catechin content detecting method in the GB/T8313-2008 tealeaves ", " GB/T 8312-2002 tea trimethyl-xanthine mensuration ", " QB2154-95 foodstuff additive tea-polyphenol " product is detected; The result is as shown in Figure 2; Can know the product catechin content up to 90.05 through quantitative Analysis, wherein the strongest EGCG content of anti-oxidant activity reaches 61.62%.The tea-polyphenol product purity is 97.82%, and theine does not detect.
Through measuring, the yield of present embodiment tea-polyphenol is 12.27%, and column chromatography is 92.30% to the recovery of tea-polyphenol.
Embodiment 2 adopts the inventive method from tealeaves, to extract no theine tea-polyphenol
3g tealeaves adds ethanolic soln (concentration 20wt%) 70ml and is heated to boiling lixiviate 30min; Cross the filter membrane in 0.45 μ m aperture; Filtrating concentrating gone up appearance to populated agarose sephadex (purchasing to GE medical treatment group) pillar; Be eluted to the flow velocity of 0.6BV/h with the ethanolic soln of 20wt% then and flow out the 1.6BV elutriant; Use the flow velocity continuation wash-out of the ethanolic soln of 67wt% with 0.6BV/h then instead, collect the elutriant of 1.6～2.1BV, elutriant concentrates, vacuum lyophilization obtains product.
Press the method testing product of embodiment 1, the result: the tea-polyphenol product purity is 98.53%, and theine does not detect, and catechin content is up to 91.20, and wherein the strongest EGCG content of anti-oxidant activity reaches 62.45%.
Through measuring, the yield of present embodiment tea-polyphenol is 11.78%, and column chromatography is 90.94% to the recovery of tea-polyphenol.
Claims (7)
1. the method for preparing no theine tea-polyphenol is characterized in that comprising the steps:
A, raw material prepare: contain theine tea-polyphenol, contain at least a in the tea leaf extract of theine, through after concentrating or being dissolved in water, filter the gained filtrate for later use;
B, gel chromatography separate: a step gained filtrating is gone up appearance to gel chromatography column; Ethanolic soln with 5～25wt% is eluted to outflow 1.3～1.7BV elutriant; It is 1.8～2.5BV that the ethanolic soln of using 50～70wt% then instead continues to be eluted to effusive elutriant, collects the elutriant of the ethanolic soln of 50～70wt%, concentrates the elutriant of collecting; Drying obtains tea-polyphenol; Wherein, the used filler of said gel permeation chromatography is sephadex lh-20 or sephadex sepharose.
2. preparation according to claim 1 does not have the method for theine tea-polyphenol; It is characterized in that: the said tea leaf extract that contains theine adopts following method to be prepared from: adopt water or ethanolic soln lixiviate tealeaves; Filter then, concentrate, obtain containing the tea leaf extract of theine.
3. preparation according to claim 2 does not have the method for theine tea-polyphenol, it is characterized in that: the concentration of the ethanolic soln of lixiviate tealeaves is 0～40wt%.
4. preparation according to claim 2 does not have the method for theine tea-polyphenol, it is characterized in that: adopt flooding tealeaves.
5. each described preparation does not have the method for theine tea-polyphenol according to claim 1～4, it is characterized in that: be filtered into membrane filtration described in a step.
6. each described preparation does not have the method for theine tea-polyphenol according to claim 1～4; It is characterized in that: the flow velocity when the b step is used the ethanolic soln wash-out of 5～25wt% is 0.5～1.0BV/h, and the flow velocity when the b step is used the ethanolic soln wash-out of 50～70wt% is 0.5～1.0BV/h.
7. each described preparation does not have the method for theine tea-polyphenol according to claim 1～4, and it is characterized in that: said b step is:
Gel chromatography separates: a step gained filtrating is gone up appearance to gel chromatography column; Be eluted to the flow velocity of 0.8BV/h with the ethanolic soln of 20wt% and flow out the 1.5BV elutriant; The ethanolic soln that uses 65wt% then continues to be eluted to effusive elutriant with the flow velocity of 0.8BV/h and is 2BV, collects the elutriant of 1.5～2BV, concentrates and collects liquid; Drying obtains tea-polyphenol.
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| CN103005112A (en) * | 2012-12-17 | 2013-04-03 | 云南柏联普洱茶庄园有限公司 | Method for reducing content of free caffeine in coffee |
| CN103012403B (en) * | 2013-01-05 | 2015-03-11 | 四川中测科技投资有限公司 | Tea leaf comprehensive utilizing and deep processing method |
| CN113498861B (en) * | 2021-07-19 | 2023-05-12 | 厦门荷蓬生物科技有限公司 | Tea source essence and preparation method thereof |
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| CN1097411A (en) * | 1994-05-19 | 1995-01-18 | 浙江医科大学 | A kind of production method of tea-polyphenol of caffein-free |
| CN100556433C (en) * | 2007-06-19 | 2009-11-04 | 华南农业大学 | Composite type high catechin tea polyphenol preparation and preparation method thereof |
| CN101099523A (en) * | 2007-07-28 | 2008-01-09 | 舒阿庆 | Method for extracting tea polyphenol from Litsea coreana |
| CN101270135B (en) * | 2008-04-24 | 2011-04-20 | 湘西自治州春天生物技术开发有限公司 | Method for removing caffeinum from tea extract of tea polyphenol containing caffeinum |
| CN101386631B (en) * | 2008-10-13 | 2012-06-06 | 湘西自治州春天生物技术开发有限公司 | Technique for extracting and separating tea polyphenol from tea-leaf |
| CN101530143B (en) * | 2009-01-12 | 2012-02-22 | 中国科学院昆明植物研究所 | Tea leaf and manufacturing method and applications thereof |
| CN102010394B (en) * | 2010-10-19 | 2012-05-02 | 浙江经贸职业技术学院 | Technology for producing low-caffeine catechin through non-solvent method |
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