CN102511598A - Method for removing alkaloid in tea by using macroporous resin - Google Patents
Method for removing alkaloid in tea by using macroporous resin Download PDFInfo
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- CN102511598A CN102511598A CN2011104218806A CN201110421880A CN102511598A CN 102511598 A CN102511598 A CN 102511598A CN 2011104218806 A CN2011104218806 A CN 2011104218806A CN 201110421880 A CN201110421880 A CN 201110421880A CN 102511598 A CN102511598 A CN 102511598A
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- tealeaves
- alkaloid
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- tea
- macroporous resin
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Abstract
The invention discloses a method for removing alkaloid in tea by using macroporous resin. The method comprises the following steps of: grinding tea leaves, mixing the ground tea leaves and boiling water, soaking, filtering, and collecting the filtrate; activating the macroporous resin, and filling the macroporous resin into a column by a wet method; regulating the pH value of the filtrate, keeping at a constant temperature, filling the filtrate into the column, performing dynamic absorption on the original tea juice by the macroporous resin, collecting and detecting the effluent, and stopping collecting the effluent till the existence of the alkaloid in the effluent is detected; and performing rotary evaporation on the collected effluent, freeze-drying the concentrate, and thus obtaining alkaloid removed tea powder. The method for removing the alkaloid in the tea by using the dynamic absorption method of the macroporous resin overcomes the defects of introduction of organic solvents such as chloroform, ethyl acetate and the like, high energy consumption and low removal rate in the prior art, and has the advantages of simple and controllable reaction conditions, environment friendliness, low cost, high alkaloid removal rate and reusability of the resin.
Description
Technical field
The present invention relates to alkaloidal method in a kind of removal tealeaves, be specifically related to a kind of alkaloidal method in the dynamic adsorbing and removing tealeaves of macroreticular resin of utilizing.
Background technology
Tea is the traditional beverages of China; Tealeaves also is the valuable cargo in China's agricultural byproducts outlet; It not only has immensely popular color; The more important thing is that it has the effect that is of illnesses and fitness, drink tea for a long time to antibiotic, reduce the body inner cholesterol, remove interior free yl, anticancer, antiatherosclerosis, prevention senile dementia etc. all have better curative effect.Yet; Alkaloid in the tealeaves particularly existence of high-load caffeine has also limited its drinking in specific crowd; As far as crowds such as neurastheniac, atherosclerotic, hypertension, pregnant woman, too much drink high-load caffeine tealeaves and can produce certain side effect.Therefore, reduce the caffeine content in the tealeaves, produce the tea product that is fit to the responsive specific crowd needs of caffeine and have the very big market space and economic worth.
Simultaneously, go alkaloid to handle, carry out deep processing tealeaves; Also be for widening the market of low and middle-grade tea; Set about from the characteristic of low and middle-grade tea,, the extracts active ingredients in the tealeaves is come out to people's different demands; Be applied to medicine, field of food and tealeaves is carried out the means of certain processed, also help realizing the unification of resource, environment, economic and social benefit.
At present, in the industry tealeaves is deviate from alkaloid, the method for extracting other active components such as Tea Polyphenols, tea polysaccharide mainly contains that extraction, deposition change the method for dissolving, the soda acid solvent takes off biological alkaline process, supercritical CO
2Gas is deviate from method etc.
(1) extraction: according to Tea Polyphenols, caffeine dissolution characteristics at solvent; Adopt extraction to reach the purpose of caffeine; Yet since extract with separate in solvent for use be chloroform, ethyl acetate etc., cause product to receive restriction, and clearance is low as medicinal or health products raw material;
(2) deposition is changeed the method for dissolving: can produce the phenomenon of complex-precipitation with metal ion according to polyphenols, earlier polyphenols centrifugalized from the tealeaves leaching liquor, sour then the commentaries on classics dissolves, and reaches and removes alkaloidal purpose; Will regulate pH in the process, bad control influences the solubility of polyphenol complex-precipitation easily, but also influences the oxidation stability of Tea Polyphenols, and recovery rate is low;
(3) the soda acid solvent takes off biological alkaline process: generally all be used in combination with organic solvent extractionprocess; Generally extraction under the organic solvent of acid condition of acid product; Alkaline impurities then salify at water; Because the amount ratio of this method acid & alkali liquid is bigger, and bringing into of organic solvent arranged, so also receive certain restriction aborning;
(4) supercritical CO
2Gas is deviate from method: utilize fluid near critical point in a certain zone; Have the behavior that balances each other unusually and transmit performance with treating the solute in the separating mixture; And the solute solvability is changed this characteristic with the pressure and temperature change reach the technology that solute separates, supercritical CO in quite wide scope
2Though it is relatively good that technology is removed alkaloidal effect,, in industrial applications, receive certain limitation because its running cost is high.
Summary of the invention
The object of the invention is to overcome the deficiency that exists in the prior art, and alkaloidal method in a kind of removal tealeaves is provided.The present invention adopts the macroreticular resin dynamic adsorption method to remove the alkaloid in the tealeaves.
The object of the invention realizes through following technical scheme:
A kind of macroreticular resin that utilizes is removed alkaloidal method in the tealeaves, may further comprise the steps:
(1) tealeaves being ground, cross 20 ~ 80 mesh sieves, is that 0.02 ~ 0.07g/mL mix with 95 ~ 100 ℃ of boiling water by mass volume ratio with tealeaves, keeps fluidized state to soak 30 ~ 60min, and suction filtration is collected filtrating, obtains tealeaves Normal juice;
(2) with after the macroreticular resin activation processing, wet method dress post;
(3) it is 4 ~ 6 and to keep temperature be 35 ~ 45 ℃ that the tealeaves Normal juice that step (1) is obtained is used pH value conditioning agent adjusting pH; With tealeaves Normal juice upper prop; Macroreticular resin dynamically adsorbs tealeaves Normal juice; Collection is flowed out liquid and is detected, and when in detecting outflow liquid, having alkaloid to exist just, stops to collect outflow liquid;
(4) the outflow liquid of step (3) being collected with the concentrate freeze drying, obtains removing alkaloidal tea powder in 55 ~ 65 ℃ of rotary evaporations.
In the step of the present invention (2), described macroreticular resin is the macroporous absorbent resin AL-1 of low pole.
In the step of the present invention (2), said activation processing may further comprise the steps: with soaked in absolute ethyl alcohol 20 ~ 28h, the absolute ethyl alcohol liquid level is higher than resin bed 8 ~ 12cm with macroreticular resin; Make the abundant swelling of resin, emit absolute ethyl alcohol, muddiness do not occur after continuing to be washed till eluate 1:5 mixes by volume with water with absolute ethyl alcohol; Be washed till with distilled water again and do not have the alcohol flavor; Suction filtration is dried then, and is subsequent use.
In the step of the present invention (3), the adsorption temp of said dynamic absorption is 35 ~ 45 ℃, and the adsorption rate of said dynamic absorption is 0.20 ~ 0.30/s.
In the step of the present invention (3), said pH value conditioning agent is a hydrochloric acid.
In the step of the present invention (3), said cryodesiccated temperature is-38 ~-42 ℃, and the time is 12 ~ 24h.
Macroreticular resin according to the invention carries out wash-out with 50% ethanol, can recycle behind the alkaloid on the removal resin.
The present invention compared with prior art has the following advantages:
(1) the present invention select low pole for use macroporous absorbent resin AL-1 as the target resin, adopt dynamic adsorption method to reach and remove alkaloidal purpose in the tealeaves, the rate of adsorption is fast, removal effect is good;
That (2) has avoided organic solvents such as chloroform, ethyl acetate in the process of the present invention brings environmental protection, environmental friendliness into;
(3) ethanol of the macroreticular resin employing 50% of the present invention's use carries out wash-out to alkaloid, can utilize once more;
(4) method of the present invention is simple to operate, and cost is low, and is pollution-free, is easy to industrialization.
The specific embodiment
In order better to understand the present invention, below in conjunction with embodiment the present invention is done detailed description further, but the scope that the present invention requires to protect is not limited thereto.
Polymeric adsorbent AL-1 purchases in Tianjin Ourui Biology Technology Co., Ltd..Need activation processing before using, concrete steps are: with soaked in absolute ethyl alcohol 20 ~ 28h, the absolute ethyl alcohol liquid level is higher than resin bed 8 ~ 12cm with macroreticular resin; Make the abundant swelling of resin, emit absolute ethyl alcohol, muddiness do not occur after continuing to be washed till eluate 1:5 mixes by volume with water with absolute ethyl alcohol; Be washed till with distilled water again and do not have the alcohol flavor; Suction filtration is dried then, and is subsequent use.
Embodiment 1
With flour mill just tealeaves ground 20 mesh sieves, in reactor, add tealeaves 30g, 98 ℃ of boiling water 750mL mix, and keep fluidized state to soak 45min, suction filtration is collected filtrating, obtains tealeaves Normal juice; After macroreticular resin AL-1 activation processing, wet method dress post; With the tealeaves Normal juice that obtains use the HCl of 2mol/L regulate pH be 4 and heating make its temperature keep 40 ℃; Upper prop; Macroreticular resin dynamically adsorbs tealeaves Normal juice, and adsorption rate is 0.20/s, and collection is flowed out liquid and detected; When in detecting outflow liquid, having alkaloid to exist just, stop to collect outflow liquid; The outflow liquid of collecting in 60 ℃ of rotary evaporations, with the concentrate freeze drying, is obtained removing alkaloidal tea powder.
(be called for short: HPLC) detect, alkaloidal clearance reaches 98.21% in the tealeaves through high performance liquid chromatography.
Embodiment 2
With flour mill just tealeaves ground 40 mesh sieves, in reactor, add tealeaves 24g, 95 ℃ of boiling water 850mL mix, and keep fluidized state to soak 60min, suction filtration is collected filtrating, obtains tealeaves Normal juice; After macroreticular resin AL-1 activation processing, wet method dress post; With the tealeaves Normal juice that obtains use the HCl of 2mol/L regulate pH be 5 and heating make its temperature keep 35 ℃; Upper prop; Macroreticular resin dynamically adsorbs tealeaves Normal juice, and adsorption rate is 0.25/s, and collection is flowed out liquid and detected; When in detecting outflow liquid, having alkaloid to exist just, stop to collect outflow liquid; The outflow liquid of collecting in 63 ℃ of rotary evaporations, with the concentrate freeze drying, is obtained removing alkaloidal tea powder.
Detect through HPLC, alkaloidal clearance reaches 98.58% in the tealeaves.
Embodiment 3
With flour mill just tealeaves ground 80 mesh sieves, in reactor, add tealeaves 35g, 100 ℃ of boiling water 700mL mix, and keep fluidized state to soak 30min, suction filtration is collected filtrating, obtains tealeaves Normal juice; After macroreticular resin AL-1 activation processing, wet method dress post; With the tealeaves Normal juice that obtains use the HCl of 2mol/L regulate pH be 6 and heating make its temperature keep 45 ℃; Upper prop; Macroreticular resin dynamically adsorbs tealeaves Normal juice, and adsorption rate is 0.30/s, and collection is flowed out liquid and detected; When in detecting outflow liquid, having alkaloid to exist just, stop to collect outflow liquid; The outflow liquid of collecting in 58 ℃ of rotary evaporations, with the concentrate freeze drying, is obtained removing alkaloidal tea powder.
Detect through HPLC, alkaloidal clearance reaches 98.17% in the tealeaves.
Claims (7)
1. one kind is utilized macroreticular resin to remove alkaloidal method in the tealeaves, it is characterized in that, may further comprise the steps:
(1) tealeaves being ground, cross 20 ~ 80 mesh sieves, is that 0.02 ~ 0.07g/mL mix with 95 ~ 100 ℃ of boiling water by mass volume ratio with tealeaves, keeps fluidized state to soak 30 ~ 60min, and suction filtration is collected filtrating, obtains tealeaves Normal juice;
(2) with after the macroreticular resin activation processing, wet method dress post;
(3) it is 4 ~ 6 and to keep temperature be 35 ~ 45 ℃ that the tealeaves Normal juice that step (1) is obtained is used pH value conditioning agent adjusting pH; With tealeaves Normal juice upper prop; Macroreticular resin dynamically adsorbs tealeaves Normal juice; Collection is flowed out liquid and is detected, and when in detecting outflow liquid, having alkaloid to exist just, stops to collect outflow liquid;
(4) the outflow liquid of step (3) being collected with the concentrate freeze drying, obtains removing alkaloidal tea powder in 55 ~ 65 ℃ of rotary evaporations.
2. method according to claim 1 is characterized in that, in the step (2), said macroreticular resin is the macroporous absorbent resin AL-1 of low pole.
3. method according to claim 2 is characterized in that, in the step (2); Said activation processing may further comprise the steps: with soaked in absolute ethyl alcohol 20 ~ 28h, the absolute ethyl alcohol liquid level is higher than resin bed 8 ~ 12cm with macroreticular resin, makes the abundant swelling of resin; Emit absolute ethyl alcohol, muddiness do not occur after continuing to be washed till eluate 1:5 mixes by volume with water with absolute ethyl alcohol, being washed till with distilled water does not have pure the flavor again; Suction filtration is dried then, and is subsequent use.
4. method according to claim 3 is characterized in that, in the step (3), the adsorption temp of said dynamic absorption is 35 ~ 45 ℃, and the adsorption rate of said dynamic absorption is 0.20 ~ 0.30/s.
5. method according to claim 3 is characterized in that, in the step (3), said pH value conditioning agent is a hydrochloric acid.
6. according to claim 4 or 5 described methods, it is characterized in that in the step (3), said cryodesiccated temperature is-38 ~-42 ℃, the time is 12 ~ 24h.
7. method according to claim 6 is characterized in that said macroreticular resin carries out wash-out with 50% ethanol, can recycle behind the alkaloid on the removal resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104218806A CN102511598A (en) | 2011-12-16 | 2011-12-16 | Method for removing alkaloid in tea by using macroporous resin |
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|---|---|---|---|
| CN2011104218806A CN102511598A (en) | 2011-12-16 | 2011-12-16 | Method for removing alkaloid in tea by using macroporous resin |
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| CN102511598A true CN102511598A (en) | 2012-06-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104642614A (en) * | 2015-03-23 | 2015-05-27 | 大闽食品（漳州）有限公司 | Method for reducing content of heavy metal ions such as arsenic and lead in instant tea |
-
2011
- 2011-12-16 CN CN2011104218806A patent/CN102511598A/en active Pending
Non-Patent Citations (4)
| Title |
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| 唐仕荣，等: "低咖啡因茶氨酸产品的精制工艺研究", 《食品科技》 * |
| 王重，等: "酚醛型吸附树脂对咖啡因和茶碱吸附性能的研究", 《高等学校化学学报》 * |
| 程冰洁，等: "FL-1大孔树脂分离纯化番石榴叶总黄酮工艺研究", 《中国中医药信息杂志》 * |
| 龚雨顺，等: "大孔吸附树脂分离茶儿茶素和咖啡因的研究", 《湖南农业大学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104642614A (en) * | 2015-03-23 | 2015-05-27 | 大闽食品（漳州）有限公司 | Method for reducing content of heavy metal ions such as arsenic and lead in instant tea |
| CN104642614B (en) * | 2015-03-23 | 2018-01-05 | 大闽食品（漳州）有限公司 | A kind of reduction instant tea includes the method for the heavy metal ion content including arsenic, lead |
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Application publication date: 20120627 |