CN105111245A - Method for extracting tea polyphenols - Google Patents
Method for extracting tea polyphenols Download PDFInfo
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- CN105111245A CN105111245A CN201510571072.6A CN201510571072A CN105111245A CN 105111245 A CN105111245 A CN 105111245A CN 201510571072 A CN201510571072 A CN 201510571072A CN 105111245 A CN105111245 A CN 105111245A
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Abstract
The invention discloses a method for extracting tea polyphenols, and belongs to the technical field of extraction methods for organic matters. The method concretely includes the steps that dried tea leaves are smashed and then screened through a screen of 30 meshes; hot water is used for digestion, then a digestion mixed solution is separated to obtain coarse extract, micro-filtration is performed on the coarse extract, ultra-filtration is performed on micro-filtration liquid, then ultra-filtration liquid is adsorbed, and finally reverse osmosis concentration is performed on the adsorbed ultra-filtration liquid to obtain the product through drying. The method is small in pollution to the environment, and the investment and energy consumption of equipment and materials involved in the method are low; in addition, the obtained tea polyphenols are high in purity and extraction rate and then have remarkable economical benefits and environmental benefits.
Description
Technical field
The present invention relates to a kind of method extracting tea-polyphenol, belong to the technical field of organism extracting method.
Background technology
The extracting method of current tea-polyphenol comprises solvent-extraction process, ion catch electron microscopy, post partition method and supercritical extraction etc.
Solvent-extraction process uses the organic solvents such as acetone, ether, methyl alcohol, ethane and trichloromethane, and not only production cost is high, and poisonous organic solvent is volatile and then cause environmental pollution; Adopt solvent-extraction process content of caffeine high simultaneously.The method that tea-polyphenol is extracted in current industrialization mainly adopts this kind.
Ion catch electron microscopy utilizes mantoquita, lead salt or aluminum chloride etc. by thick tea through water extraction, and ion precipitation extracts the tea-polyphenol in tealeaves; But containing the heavy metal poisonous to human body in the solution adopted, and then there is great harm to human body and environment.
Post is separated preparation method and mainly adds the moieties that stopping composition carries out as adsorptive type resin in adsorption and desorption solution.Adopt the tea-polyphenol extracted in this way in tealeaves, it generally adopts the materials such as lipophilic gel; And lipophilic gel cost is high, also need with multiple a large amount of organic solvent during this external drip washing, this obvious improper suitability for industrialized production tea-polyphenol.
In addition, also there is the defects such as percentage extraction is low, facility investment large, demand strict technology in supercritical extraction.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of method that cost is low, pollute little, that extraction yield is high extraction tea-polyphenol, it is realized primarily of following technical scheme.
Methods of Extraction of Tea-polyphenols of the present invention, it comprises the following steps:
1) dry tealeaves was pulverized 30 mesh sieves and was obtained tea powder;
2) above-mentioned tea powder with hot water lixiviate 2 ~ 3 times;
3) carry out merging to obtain crude extract after being separated the above-mentioned mixed solution of lixiviate several times;
4) micro-filtration is carried out to crude extract and obtain micro-filtrate;
5) ultrafiltration is carried out to micro-filtrate and obtain ultrafiltrated;
6) ultrafiltrated is adsorbed, with gac or acidic white earth absorption caffeine;
7) carry out reverse osmosis concentration to the ultrafiltrated after absorption and obtain concentrated solution, then drying obtains product.
Particularly, above-mentioned steps 1) be to expand lixiviate area, improve leaching yield.
Particularly, above-mentioned steps 2) hot water extraction to carry out being separated also be to improve leaching yield.
Further, above-mentioned steps 2) extracting technology condition: solid-liquid ratio 1 ︰ 15-25, lixiviate 2-3 time, water temp 80-90 DEG C, each extraction time 20-30min.
Further, above-mentioned steps 3) separation process conditions: 300 mesh sieve centrifugings obtain crude extract, and the tea grounds fermentation obtained is as fertilizer.
Particularly, above-mentioned steps 4) be to remove minute solid particles and larger molecular organics.
Further, above-mentioned steps 4) micro-filtration processing condition: the removal of impurities of 0.2um ceramic microfiltration membrane obtains micro-filtrate, and the pressure of micro-filtration is 0.2MPa, and the temperature of micro-filtration operation is 25 DEG C.
Particularly, above-mentioned steps 5) be to remove larger molecular organics further.
Further, above-mentioned steps 5) ultrafiltration technology condition: 100-200kDa membranous system, pressure-controlling is 0.4MPa, and temperature is 25 DEG C, and wherein average flux is 50L/m
2h, cycles of concentration 14, solid content yield 82%, solid content>=2.5%.
Particularly, above-mentioned steps 6) adsorption operations be to remove the materials such as caffeine.
Further, above-mentioned steps 6) in, when adopting gac, activated carbon dosage 45g/L, is wherein incubated 40 DEG C and adsorbs 2h; When adopting acidic white earth, acidic white earth consumption 30g/L, room temperature absorption 40min, absorption number of times 3 times, stirring velocity 120r/min.
Particularly, above-mentioned steps 7) be concentration in order to improve tea-polyphenol in solution.
Further, above-mentioned steps 7) adopt reverse osmosis membrane ultrafiltration concentration liquid, concentrated solution carries out drying and obtains product, and permeate is that pure water can be recycled.Above-mentioned concentrated solution drying treatment adopts spraying dry or lyophilize to obtain finished product tea-polyphenol.
Further, the product polyphenol content (TP) >=85% that aforesaid method of the present invention obtains is adopted, tea polysaccharide and theanine total amount >=11.3%, caffeine < 0.5%.
Beneficial effect of the present invention: not with an organic solvent and heavy metal ion, therefore there is not organic solvent residual, also heavy metal free ion residues, Product Safety is good, and environmental pollution is little for technical scheme disclosed by the invention.Aforesaid operations temperature of the present invention is low, need not use organism, preserves the activity of tea-polyphenol to greatest extent.In addition, few, the equipment of sewage discharge of the present invention and material investment is low, energy consumption is low; Meanwhile, the activity of the tea-polyphenol obtained is strong, so technical scheme of the present invention has obvious economic benefit and environmental benefit.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.In embodiment, concrete involved condition and parameter should not as the restrictions of technical solution of the present invention, and any improvement done on the basis of the above and change all belong to the protection domain of technical solution of the present invention.
embodiment 1
The tealeaves 300g of drying was pulverized 30 mesh sieves; Then be lixiviate in 85 DEG C in water temperature, solid-liquid ratio is 1 ︰ 17, lixiviate 27min, 300 mesh sieve centrifugings; And then to drop into solid-liquid ratio be 1 ︰ 21, temperature is lixiviate 35min in the water of 90 DEG C, 300 mesh sieve centrifugings; Collect twice extracted filtrate and obtain crude extract, the tea grounds fermentation of gained is as fertilizer.Then to the removal of impurities of crude extract 0.2um ceramic microfiltration membrane to obtain micro-filtrate, wherein pressure is, 0.2MPa, and micro-filtration temperature is 25 DEG C; Then carry out ultrafiltration to micro-filtrate, ultrafiltration technology condition: 100kDa ultrafiltration membrane system, wherein pressure is 0.4MPa, and it is 25 DEG C that temperature controls, average flux 50L/m
2.h, cycles of concentration 14, solid content yield 82%, gained ultrafiltrated adsorbs, and adopts gac or acidic white earth, wherein activated carbon dosage 45g/L, is incubated 40 DEG C and adsorbs 2h in adsorption process; Finally carry out reverse osmosis membrane to the ultrafiltrated after absorption to concentrate, concentrated solution obtains product by lyophilize, and above-mentioned permeate is that pure water can be recycled.In product obtained above, polyphenol content is 85.7%, content of tea polysaccharide 6.2%, theanine content 5.3%, content of caffeine 0.4%, surplus be water and impurity.
embodiment 2
Dry tealeaves 500g is pulverized the tea powder with hot water that 30 mesh sieves obtain excessively afterwards and carry out lixiviate, solid-liquid ratio 1 ︰ 18 of first time lixiviate, water temperature 80 DEG C, lixiviate 25min, 300 mesh sieve centrifugings; The solid-liquid ratio of second time lixiviate is 1 ︰ 20, and water temperature is 85 DEG C, lixiviate 20min, 300 mesh sieve centrifugings; During third time lixiviate, solid-liquid ratio is 1 ︰ 22, and water temperature is 80 DEG C, extraction time 10min, 300 mesh sieve centrifugings; The extracted filtrate merging above-mentioned three times obtains crude extract, finally obtains tea grounds fermentation and makees fertilizer; Then carry out micro-filtration to crude extract, micro-filtration processing condition: the removal of impurities of 0.2um ceramic microfiltration membrane, in microfiltration process, pressure is 0.2MPa, and the temperature of micro-filtration is 25 DEG C; Then carry out ultrafiltration to micro-filtrate, ultrafiltration technology condition: 200kDa ultrafiltration membrane system, the pressure-controlling of wherein ultrafiltration is 0.4MPa, and the temperature of ultrafiltration is 25 DEG C, wherein average flux 50L/m
2h, cycles of concentration 14, solid content yield 82%, then adsorbs ultrafiltrated, and adopt acidic white earth, acidic white earth consumption 30g/L, it is 40min that room temperature adsorbs each adsorption time, absorption number of times 3 times, stirring velocity 120r/min; Finally carry out reverse osmosis concentration to the ultrafiltrated after absorption, with reverse osmosis membrane ultrafiltration concentration liquid, concentrated solution carries out drying and obtains product; Wherein obtain tea-polyphenol by lyophilize, TP content is 85.5%, content of tea polysaccharide 6.3%, theanine content 5.4%, content of caffeine 0.3%, surplus be water and impurity.
Claims (8)
1. extract a method for tea-polyphenol, it is characterized in that: comprise the following steps:
1) dry tealeaves is crossed 30 mesh sieves after pulverizing and is obtained tea-leaf power;
2) the tea-leaf power hot water pulverized carries out lixiviate 2 ~ 3 times;
3) separating step 2) vat liquor and carry out merging to obtain crude extract;
4) micro-filtration is carried out to crude extract and obtain micro-filtrate;
5) ultrafiltration is carried out to micro-filtrate and obtain ultrafiltrated;
6) ultrafiltrated is adsorbed, adopt gac or acidic white earth absorption caffeine;
7) reverse osmosis concentrated dry the product that contracts is carried out to the ultrafiltrated after absorption.
2. a kind of method extracting tea-polyphenol according to claim 1, is characterized in that: described step 2) extracting technology condition be: solid-liquid ratio 1 ︰ 15-25, lixiviate 2-3 time, extraction temperature 80-90 DEG C, each extraction time 20-30min.
3. a kind of method extracting tea-polyphenol according to claim 1, is characterized in that: described step 3) separation process conditions: 300 mesh sieve centrifugings obtain crude extract, and fertilizer is made in the fermentation of the tea grounds that obtains.
4. a kind of method extracting tea-polyphenol according to claim 1, is characterized in that: described step 4) micro-filtration processing condition be: the removal of impurities of 0.2um ceramic microfiltration membrane, wherein pressure controls as 0.2MPa, and micro-filtration temperature is 25 DEG C.
5. a kind of method extracting tea-polyphenol according to claim 1, is characterized in that: described step 5) ultrafiltration technology condition: 100-200kDa membranous system, ultrafiltration pressure is 0.4MPa, and ultrafiltrate temperature is 25 DEG C, average flux 50L/m
2h, cycles of concentration 14.
6. a kind of method extracting tea-polyphenol according to claim 1, is characterized in that: described step 6) when using charcoal absorption, activated carbon dosage 45g/L, is wherein incubated 40 DEG C and adsorbs 2h.
7. a kind of method extracting tea-polyphenol according to claim 1, is characterized in that: described step 6) when adsorbing with acidic white earth, acidic white earth consumption 30g/L, absorption number of times 3 times, each room temperature absorption 40min, stirring velocity 120r/min.
8. a kind of method extracting tea-polyphenol according to claim 1, is characterized in that: described step 7) adopt concentrated solution spraying or lyophilize to obtain tea-polyphenol, polyphenol content >=85%.
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| CN201510571072.6A CN105111245A (en) | 2015-09-10 | 2015-09-10 | Method for extracting tea polyphenols |
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| CN201510571072.6A CN105111245A (en) | 2015-09-10 | 2015-09-10 | Method for extracting tea polyphenols |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105968146A (en) * | 2016-05-11 | 2016-09-28 | 张铰铣 | Tea polyphenol production process for producing plurality of products by one time of feeding |
| CN107602628A (en) * | 2017-08-18 | 2018-01-19 | 合肥丰洁生物科技有限公司 | A kind of Green Tea Polyphenols UF membrane process for purification |
| CN113317375A (en) * | 2021-06-04 | 2021-08-31 | 杭州浙大百川生物食品技术有限公司 | Green tea concentration method |
Citations (3)
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| CN1634914A (en) * | 2004-11-23 | 2005-07-06 | 三达膜科技（厦门）有限公司 | Method for producing high pure tea polyphenol with low caffeine |
| CN101475606A (en) * | 2009-01-15 | 2009-07-08 | 浙江大学 | Process for extracting tea polyphenol in tea |
| CN101508690A (en) * | 2009-03-17 | 2009-08-19 | 林峰 | Novel methods for simultaneously extracting tea polyphenol, tea polysaccharide and caffeinum from tea |
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2015
- 2015-09-10 CN CN201510571072.6A patent/CN105111245A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1634914A (en) * | 2004-11-23 | 2005-07-06 | 三达膜科技（厦门）有限公司 | Method for producing high pure tea polyphenol with low caffeine |
| CN101475606A (en) * | 2009-01-15 | 2009-07-08 | 浙江大学 | Process for extracting tea polyphenol in tea |
| CN101508690A (en) * | 2009-03-17 | 2009-08-19 | 林峰 | Novel methods for simultaneously extracting tea polyphenol, tea polysaccharide and caffeinum from tea |
Non-Patent Citations (2)
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| 姜绍通，侯晨晔: "基于膜分离的茶多酚绿色制备方法研究", 《食品科技》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105968146A (en) * | 2016-05-11 | 2016-09-28 | 张铰铣 | Tea polyphenol production process for producing plurality of products by one time of feeding |
| CN107602628A (en) * | 2017-08-18 | 2018-01-19 | 合肥丰洁生物科技有限公司 | A kind of Green Tea Polyphenols UF membrane process for purification |
| CN113317375A (en) * | 2021-06-04 | 2021-08-31 | 杭州浙大百川生物食品技术有限公司 | Green tea concentration method |
| CN113317375B (en) * | 2021-06-04 | 2022-07-19 | 杭州浙大百川生物食品技术有限公司 | Green tea concentration method |
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Application publication date: 20151202 |