CN102225122A - Caffeine-free tea polyphenol and preparation method thereof - Google Patents
Caffeine-free tea polyphenol and preparation method thereof Download PDFInfo
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- CN102225122A CN102225122A CN 201110153466 CN201110153466A CN102225122A CN 102225122 A CN102225122 A CN 102225122A CN 201110153466 CN201110153466 CN 201110153466 CN 201110153466 A CN201110153466 A CN 201110153466A CN 102225122 A CN102225122 A CN 102225122A
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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 caffeine tea polyphenols and preparation method thereof, belong to the separation and Extraction field.
Background technology
Tea polyphenols is the important active component of tea Ye Zhongyi class, content is generally accounting for 18%～36% of dry weight of tea leaves, it is a kind of natural antioxidant, can be widely used in industries such as food, medicine, health product and cosmetics, also possesses blood fat reducing and blood glucose simultaneously, blood pressure lowering and cholesterol, functions such as arteriosclerosis, mutation and anticancer change, defying age, antioxidation, and be used for the multiple disease of clinical treatment.
At present, the method for preparing tea polyphenols mainly contains solvent extraction, resin absorption partition method and supercritical extraction.Solvent extraction is that tea polyphenols is produced the technology that the most generally adopts at present, its yield height, and cost is low, but product quality is lower, content of caffeine height, organic solvent residual height, Environmental costs height.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 polyphenols.Supercritical extraction with an organic solvent also can not get the low-caffeine tea polyphenols, but product impurity is many, product purity is not high, and equipment input and maintenance cost are too high, operating condition is strict, realize that suitability for industrialized production also has certain difficulty.
Tea polyphenols purity height, particularly caffeine and catechin content have directly determined the quality and the purposes of product.Therefore, no caffeine of preparation and the high tea polyphenols 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 caffeine tea polyphenols.
The method that the present invention prepares no caffeine tea polyphenols comprises the steps:
A, raw material prepare: contain caffeine tea polyphenols, contain at least a in the Folium Camelliae sinensis extract of caffeine, through concentrating or being dissolved in water (if raw material is a solution, then concentrate, if raw material is solid or semisolid, then be dissolved in water,, preferably prepare the solution of high concentration for the ease of chromatography, 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 filtrate is gone up sample to gel chromatography column, alcoholic solution with 5～25wt% is eluted to outflow 1.3～1.7BV eluent, it is 1.8～2.5BV that the alcoholic solution of using 50～70wt% then instead continues to be eluted to effusive eluent, collect the eluent of the alcoholic solution of 50～70wt%, concentrate the eluent of collecting, dry (preferred vacuum lyophilization) obtains tea polyphenols; Wherein, the used filler of described gel permeation chromatography is sephadex lh-20 or cross-linking dextran agarose gel.
Wherein, the tea polyphenols that contains caffeine in the above-mentioned a step, the Folium Camelliae sinensis extract that contains caffeine can adopt the commercially available prod, also can prepare voluntarily.As the Folium Camelliae sinensis extract that contains caffeine can adopt following method to be prepared from: adopt water or alcoholic solution lixiviate Folium Camelliae sinensis, filter then, concentrate, obtain containing the Folium Camelliae sinensis extract of caffeine.
Wherein, when water or alcoholic solution lixiviate Folium Camelliae sinensis, the consumption of water or alcoholic solution is that conventional amount used gets final product, further, the consumption of water or alcoholic solution is preferably 6～70 times of Folium Camelliae sinensis weight, and the consumption of water or alcoholic solution most preferably is 15～30 times of Folium Camelliae sinensis weight.
Wherein, the alcoholic solution of concentration comprises that straight alcohol solution (being the above alcoholic solution of 95wt%) may be used to the lixiviate of Folium Camelliae sinensis arbitrarily, and in order to reduce cost, the concentration of alcoholic solution 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 Folium Camelliae sinensis because water (boiling water) lixiviate Folium Camelliae sinensis does not have notable difference with comparing with tea polyphenols in the alcoholic solution lixiviate Folium Camelliae sinensis.
Wherein, when preparation contains the Folium Camelliae sinensis extract of caffeine, can adopt conventional method to concentrate, method for concentration 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 alcoholic solution eluting of 5～25wt% is preferably 0.5～1.0BV/h, and the flow velocity of b step during with the alcoholic solution eluting 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 filtrate is gone up sample to gel chromatography column, be eluted to the flow velocity of 0.8BV/h with the alcoholic solution of 20wt% and flow out the 1.5BV eluent, continuing to be eluted to effusive eluent with the alcoholic solution of 65wt% with the flow velocity of 0.8BV/h then is 2BV, collects the eluent of 1.5～2BV, concentrates and collects liquid, drying obtains tea polyphenols.
Wherein, the used filler of the described gel permeation chromatography of above-mentioned b step is preferably sephadex lh-20.
The present invention also provides by the prepared no caffeine tea polyphenols of said method.
The inventive method is simple to operate, the production efficiency height, and economic environmental protection, 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 polyphenols 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 antioxidant activity is more than 60%.The present invention has broad application prospects for tea polyphenols production high-quality, high added value provides a kind of new selection
Description of drawings
Fig. 1 prepares the chromatogram of tea polyphenols for column chromatography for separation, and wherein, peak A is a tea polyphenols;
Fig. 2 is the high-efficient liquid phase analysis chromatogram, and among the figure, figure (A) is the chromatogram of product; Figure (B) is the chromatogram of Folium Camelliae sinensis extract, and figure (C) is the chromatogram of Folium Camelliae sinensis biochemical component standard substance.
The specific embodiment
The method that the present invention prepares no caffeine tea polyphenols comprises the steps:
A, raw material prepare: contain caffeine tea polyphenols, contain at least a in the Folium Camelliae sinensis extract of caffeine, through concentrating or being dissolved in water (if raw material is a solution, then concentrate, if raw material is solid or semisolid, then be dissolved in water,, preferably prepare the solution of high concentration for the ease of chromatography, 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 filtrate is gone up sample to gel chromatography column, alcoholic solution with 5～25wt% is eluted to outflow 1.3～1.7BV eluent, it is 1.8～2.5BV that the alcoholic solution of using 50～70wt% then instead continues to be eluted to effusive eluent, collect the eluent of the alcoholic solution of 50～70wt%, concentrate the eluent of collecting, dry (preferred vacuum lyophilization) obtains tea polyphenols; Wherein, the used filler of described gel permeation chromatography is sephadex lh-20 or cross-linking dextran agarose gel.
Wherein, the tea polyphenols that contains caffeine in the above-mentioned a step, the Folium Camelliae sinensis extract that contains caffeine can adopt the commercially available prod, also can prepare voluntarily.As the Folium Camelliae sinensis extract that contains caffeine can adopt following method to be prepared from: adopt water or alcoholic solution lixiviate Folium Camelliae sinensis, filter then, concentrate, obtain containing the Folium Camelliae sinensis extract of caffeine.
Wherein, when water or alcoholic solution lixiviate Folium Camelliae sinensis, the consumption of water or alcoholic solution is that conventional amount used gets final product, further, the consumption of water or alcoholic solution is preferably 6～70 times of Folium Camelliae sinensis weight, and the consumption of water or alcoholic solution most preferably is 15～30 times of Folium Camelliae sinensis weight.
Wherein, the alcoholic solution of concentration comprises that straight alcohol solution (being the above alcoholic solution of 95wt%) may be used to the lixiviate of Folium Camelliae sinensis arbitrarily, and in order to reduce cost, the concentration of alcoholic solution 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 Folium Camelliae sinensis because water (boiling water) lixiviate Folium Camelliae sinensis does not have notable difference with comparing with tea polyphenols in the alcoholic solution lixiviate Folium Camelliae sinensis.
Wherein, when preparation contains the Folium Camelliae sinensis extract of caffeine, can adopt conventional method to concentrate, method for concentration 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 alcoholic solution eluting of 5～25wt% is preferably 0.5～1.0BV/h, and the flow velocity of b step during with the alcoholic solution eluting 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 filtrate is gone up sample to gel chromatography column, be eluted to the flow velocity of 0.8BV/h with the alcoholic solution of 20wt% and flow out the 1.5BV eluent, continuing to be eluted to effusive eluent with the alcoholic solution of 65wt% with the flow velocity of 0.8BV/h then is 2BV, collects the eluent of 1.5～2BV, concentrates and collects liquid, drying obtains tea polyphenols.
Wherein, the used filler of the described gel permeation chromatography of above-mentioned b step is preferably sephadex lh-20.
The present invention also provides by the prepared no caffeine tea polyphenols of said method.
Below in conjunction with embodiment the specific embodiment of the present invention is further described, does not therefore limit the present invention among the described scope of embodiments.
Embodiment 1 adopts the inventive method to extract no caffeine tea polyphenols from Folium Camelliae sinensis
3g Folium Camelliae sinensis adds boiling water 50ml lixiviate 30min, cross the filter membrane in 0.45 μ m aperture, filtrate concentrating gone up sample to populated sephadex lh-20 (purchasing to GE medical treatment group) pillar, be eluted to the flow velocity of 0.8BV/h with the alcoholic solution of 20wt% then and flow out the 1.5BV eluent, use the flow velocity continuation eluting of the alcoholic solution of 65wt% then instead with 0.8BV/h, collect the eluent of 1.5～2BV, eluent concentrates, vacuum lyophilization obtains product.
The chromatogram that column chromatography for separation prepares tea polyphenols as shown in Figure 1, wherein, peak A is tea polyphenols.According to standard " tea polyphenols and catechin content detecting method in the GB/T8313-2008 Folium Camelliae sinensis ", " GB/T 8312-2002 tea caffeine mensuration ", " QB2154-95 food additive tea polyphenols " product is detected, the result as shown in Figure 2, the product catechin content is up to 90.05 as can be known by quantitative Analysis, and wherein the strongest EGCG content of antioxidant activity reaches 61.62%.The tea polyphenols product purity is 97.82%, and caffeine does not detect.
After measured, the yield of present embodiment tea polyphenols is 12.27%, and column chromatography is 92.30% to the response rate of tea polyphenols.
Embodiment 2 adopts the inventive method to extract no caffeine tea polyphenols from Folium Camelliae sinensis
3g Folium Camelliae sinensis adds alcoholic solution (concentration 20wt%) 70ml and is heated to boiling lixiviate 30min, cross the filter membrane in 0.45 μ m aperture, filtrate concentrating gone up sample to populated agarose sephadex (purchasing to GE medical treatment group) pillar, be eluted to the flow velocity of 0.6BV/h with the alcoholic solution of 20wt% then and flow out the 1.6BV eluent, use the flow velocity continuation eluting of the alcoholic solution of 67wt% then instead with 0.6BV/h, collect the eluent of 1.6～2.1BV, eluent concentrates, vacuum lyophilization obtains product.
Press the method testing product of embodiment 1, the result: the tea polyphenols product purity is 98.53%, and caffeine does not detect, and catechin content is up to 91.20, and wherein the strongest EGCG content of antioxidant activity reaches 62.45%.
After measured, the yield of present embodiment tea polyphenols is 11.78%, and column chromatography is 90.94% to the response rate of tea polyphenols.
Claims (8)
1. the method for preparing no caffeine tea polyphenols is characterized in that comprising the steps:
A, raw material prepare: contain caffeine tea polyphenols, contain at least a in the Folium Camelliae sinensis extract of caffeine, through after concentrating or being dissolved in water, filter the gained filtrate for later use;
B, gel chromatography separate: a step gained filtrate is gone up sample to gel chromatography column, alcoholic solution with 5～25wt% is eluted to outflow 1.3～1.7BV eluent, it is 1.8～2.5BV that the alcoholic solution of using 50～70wt% then instead continues to be eluted to effusive eluent, collect the eluent of the alcoholic solution of 50～70wt%, concentrate the eluent of collecting, drying obtains tea polyphenols; Wherein, the used filler of described gel permeation chromatography is sephadex lh-20 or cross-linking dextran agarose gel.
2. preparation according to claim 1 does not have the method for caffeine tea polyphenols, it is characterized in that: the described Folium Camelliae sinensis extract that contains caffeine adopts following method to be prepared from: adopt water or alcoholic solution lixiviate Folium Camelliae sinensis, filter then, concentrate, obtain containing the Folium Camelliae sinensis extract of caffeine.
3. preparation according to claim 2 does not have the method for caffeine tea polyphenols, it is characterized in that: the concentration of the alcoholic solution of lixiviate Folium Camelliae sinensis is 0～40wt%.
4. preparation according to claim 2 does not have the method for caffeine tea polyphenols, it is characterized in that: adopt flooding Folium Camelliae sinensis.
5. each described preparation does not have the method for caffeine tea polyphenols 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 caffeine tea polyphenols according to claim 1～5, it is characterized in that: the flow velocity of b step during with the alcoholic solution eluting of 5～25wt% is 0.5～1.0BV/h, and the flow velocity of b step during with the alcoholic solution eluting of 50～70wt% is 0.5～1.0BV/h.
7. each described preparation does not have the method for caffeine tea polyphenols according to claim 1～6, and it is characterized in that: described b step is:
Gel chromatography separates: a step gained filtrate is gone up sample to gel chromatography column, be eluted to the flow velocity of 0.8BV/h with the alcoholic solution of 20wt% and flow out the 1.5BV eluent, continuing to be eluted to effusive eluent with the alcoholic solution of 65wt% with the flow velocity of 0.8BV/h then is 2BV, collect the eluent of 1.5～2BV, concentrate and collect liquid, drying obtains tea polyphenols.
8. by the prepared no caffeine tea polyphenols of each described method of claim 1～7.
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Cited By (3)
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| CN103012403A (en) * | 2013-01-05 | 2013-04-03 | 四川中测科技投资有限公司 | Tea leaf comprehensive utilizing and deep processing method |
| 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 |
| CN113498861A (en) * | 2021-07-19 | 2021-10-15 | 厦门荷蓬生物科技有限公司 | Tea extract and preparation method thereof |
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| CN103012403A (en) * | 2013-01-05 | 2013-04-03 | 四川中测科技投资有限公司 | Tea leaf comprehensive utilizing and deep processing method |
| 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 |
| CN113498861A (en) * | 2021-07-19 | 2021-10-15 | 厦门荷蓬生物科技有限公司 | Tea extract and preparation method thereof |
| 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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