CN100539859C - From tealeaves, extract the method for Tea Polyphenols - Google Patents
From tealeaves, extract the method for Tea Polyphenols Download PDFInfo
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- CN100539859C CN100539859C CNB2006101552762A CN200610155276A CN100539859C CN 100539859 C CN100539859 C CN 100539859C CN B2006101552762 A CNB2006101552762 A CN B2006101552762A CN 200610155276 A CN200610155276 A CN 200610155276A CN 100539859 C CN100539859 C CN 100539859C
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- tea
- tea polyphenols
- tealeaves
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- polyphenols
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- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 57
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000284 extract Substances 0.000 title claims description 5
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 claims abstract description 52
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229960001948 caffeine Drugs 0.000 claims abstract description 26
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 15
- 229920005989 resin Polymers 0.000 claims abstract description 15
- 239000012528 membrane Substances 0.000 claims abstract description 10
- 239000003463 adsorbent Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims abstract description 9
- 238000001179 sorption measurement Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000012141 concentrate Substances 0.000 claims abstract description 6
- 229920002678 cellulose Polymers 0.000 claims abstract description 5
- 239000001913 cellulose Substances 0.000 claims abstract description 5
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 5
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 3
- 235000013616 tea Nutrition 0.000 claims description 64
- 244000269722 Thea sinensis Species 0.000 claims description 26
- 235000009569 green tea Nutrition 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 7
- 238000010828 elution Methods 0.000 claims description 6
- 229920000620 organic polymer Polymers 0.000 claims description 4
- 241000609240 Ambelania acida Species 0.000 claims description 2
- 239000010905 bagasse Substances 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 229920002492 poly(sulfone) Polymers 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims description 2
- 239000010902 straw Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 235000013305 food Nutrition 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 239000002910 solid waste Substances 0.000 abstract description 2
- 241001122767 Theaceae Species 0.000 abstract 2
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000003809 water extraction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 description 8
- 235000005487 catechin Nutrition 0.000 description 8
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 8
- 229950001002 cianidanol Drugs 0.000 description 8
- 239000003480 eluent Substances 0.000 description 8
- 238000000746 purification Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 150000001455 metallic ions Chemical class 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003810 ethyl acetate extraction Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000011165 process development Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Separation Using Semi-Permeable Membranes (AREA)
- Tea And Coffee (AREA)
Abstract
The invention discloses the method for from tealeaves, extracting Tea Polyphenols, with the tea juice of pulverizing tea behind water extraction, successively through the film coarse filtration, film ultrafiltration, membrane reverse osmosis concentrate to be carried densely, passes through nonpolar macroporous adsorption resin again, the ethanolic solution wash-out, the Tea Polyphenols solution that obtains purifying; This solution is adsorbed by cellulose adsorbent again, remove caffeine, with Different concentrations of alcohol solution gradient wash-out, concentrate and reclaim ethanol, drying gets the Tea Polyphenols product.The inventive method is simple to operate, and the Tea Polyphenols of production does not contain organic dissolvent residual (except the ethanol), meets the requirement of pollution-free food and pharmaceutical raw material.The discharge of no solid waste in the production process, the most of recyclable utilization again of process water, sewage flow rate is less, compliance with environmental protection requirements.
Description
Technical field
The present invention relates to extract the method for Tea Polyphenols from tealeaves.
Background technology
Because the medicinal efficacy of Tea Polyphenols or catechin and health care more and more receive popular concern, the technological process development in recent years of extracting Tea Polyphenols or catechin from tealeaves is very fast.Tea Polyphenols or catechin extraction process from tealeaves has formed having of production capacity: use organic solvent extractionprocess; 3 kinds of precipitation by metallic ion method and resin adsorption methods, though precipitation by metallic ion method product purity height wherein, but complicated operation, recovery rate is low, at present industrially be eliminated, though resin adsorption method extracts the yield height, energy consumption is also low, but caffeine content height in the product can only be done crude product Tea Polyphenols product, at present in order to obtain polyphenol content＞98%, the Tea Polyphenols product of caffeine content≤3.0%, all adopt leaching---solvent extraction, this method flow is simple to operate, and yield 6-9% is not low yet, shortcoming is to have introduced chloroform or chlorinated organics removal caffeine and ethyl acetate extraction technology in the flow process, the former is poisonous organic solvent, though also useful at present acid solution such as citric acid etc. are removed caffeine technology, is inevitable with the extraction of organic solvent ethyl acetate.Ethyl acetate remains in and all can bring the healthy adverse influence to the people in the product, if further purified the raw material of catechin as medicine, then the residual of ethyl acetate will bring fatal influence.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, extracts the method for Tea Polyphenols from tealeaves without organic solvent (except the ethanol).
The method of from tealeaves, extracting Tea Polyphenols of the present invention, its step is as follows:
1) will pulverize green tea and carry out counter-current extraction, remove tea grounds through mechanical filter;
2) removing tea juice behind the tea grounds successively through the film coarse filtration, the film ultrafiltration, membrane reverse osmosis concentrate carry dense;
3) will carry tea juice after dense with the 1-6BV/hr flow velocity by nonpolar macroporous adsorption resin, with ethanolic solution wash-out from the resin, the Tea Polyphenols solution that obtains purifying;
4) the Tea Polyphenols solution of Ti Chuning by cellulose adsorbent, through the adsorbing and removing caffeine, is used the ethanolic solution gradient elution of 20～90% concentration with the 1-6BV/hr flow velocity again, concentrates to reclaim ethanol, and drying gets the Tea Polyphenols product.
Among the present invention, the coarse filtration film of concentrated tea juice can be organic polymer tubular membrane or a ceramic pipe type film of removing 10～200,000 Dalton molecular weights.Milipore filter can adopt the organic polymer tubular membrane of removing 20,000～100,000 Dalton molecular weights.Reverse osmosis membrane can be the polysulfones rolling NF membrane that sees through 200 dalton molecules.
Among the present invention, said cellulose adsorbent can be trees, straw, corncob or bagasse.
In order to leach more Tea Polyphenols, the water temperature that counter-current extraction is pulverized green tea is controlled at 70～80 ℃.
Beneficial effect of the present invention is:
1) the inventive method is simple to operate, and the Tea Polyphenols of production does not contain organic dissolvent residual (except the ethanol), meets the requirement of pollution-free food and pharmaceutical raw material.
2) product of different Tea Polyphenols and caffeine content specification can be produced by regulating operating parameter, to adapt to the needs of fluctuation of price, polyphenol content＞98% can be produced, the smart Tea Polyphenols product of caffeine content≤3.0%.
3) discharge of no solid waste in the production process of the present invention, the most of recyclable utilization again of process water, sewage flow rate is less, compliance with environmental protection requirements.
4) the present invention is raw material with tealeaves, can obtain other accessory substances except that Tea Polyphenols simultaneously, as the tea polysaccharide raw material, and the caffeine raw material, particularly tea grounds can be used as organic composite fertilizer through biological treatment.
Description of drawings
Fig. 1 is the process chart of the inventive method.
The specific embodiment
Example 1
With old green tea 50 grams in Mianyang, Sichuan, with tea=weight ratio lixiviate in 1: 20, water temperature keeps 70 ℃ of lixiviates 30 minutes, through filtrations at different levels and carry dense after, get filtered fluid 200ml, Tea Polyphenols concentration is about 10mg/ml in the tealeaves, pass through 25mm * 300mm nonpolar macroporous adsorption resin with the 1BV/hr flow velocity, Tea Polyphenols and caffeine have 90% to be adsorbed on the resin approximately, obtain the high purification Tea Polyphenols solution of caffeine content with 80% ethanolic solution wash-out again, get this purification Tea Polyphenols solution 100ml by 25mm * 250mm lignocellulosic adsorbent post, the operation flow velocity be 1BV/hr when flowing through Tea Polyphenols be adsorbed, caffeine is discharged by flowing through liquid, uses 40% again, 60% ethanolic solution gradient elution, flow velocity is 1BV/hr, and eluent reclaims ethanol, and eluent is concentrated simultaneously, final drying obtains product: polyphenol content 112% catechin 60% caffeine content 1.13% yield 6.5%.
Example 2
With old green tea 50 grams in Mianyang, Sichuan, with tea=weight ratio lixiviate in 1: 10, water temperature keeps 80 ℃ of lixiviates 40 minutes, through filtrations at different levels and carry dense after, get filtered fluid 200ml, Tea Polyphenols concentration is about 20mg/ml in the tealeaves, pass through 25mm * 300mm nonpolar macroporous adsorption resin with the 6BV/hr flow velocity, Tea Polyphenols and caffeine have 80% to be adsorbed on the resin approximately, obtain the high purification Tea Polyphenols solution of caffeine content with 70% ethanolic solution wash-out again, get this purification Tea Polyphenols solution 100ml by 25mm * 250mm lignocellulosic adsorbent post, the operation flow velocity be 6BV/hr when flowing through Tea Polyphenols be adsorbed, caffeine is discharged by flowing through liquid, use 20% again, 40%, 60% ethanolic solution gradient elution, flow velocity are 6BV/hr, eluent reclaims ethanol, eluent is concentrated simultaneously, and final drying obtains product: polyphenol content 102.8% catechin 61% caffeine content 1.53% yield 6.99%.
Example 3
With old green tea 50 grams in Mianyang, Sichuan, with tea=weight ratio lixiviate in 1: 20, water temperature keeps 70 ℃ of lixiviates 30 minutes, through filtrations at different levels and carry dense after, get filtered fluid 200ml, Tea Polyphenols concentration is about 10mg/ml in the tealeaves, pass through 25mm * 300mm nonpolar macroporous adsorption resin with the 4BV/hr flow velocity, Tea Polyphenols and caffeine have 85% to be adsorbed on the resin approximately, obtain the high purification Tea Polyphenols solution of caffeine content with 70% ethanolic solution wash-out again, get this purification Tea Polyphenols solution 100ml by 25mm * 250mm lignocellulosic adsorbent post, the operation flow velocity be 4BV/hr when flowing through Tea Polyphenols be adsorbed, caffeine is discharged by flowing through liquid, use 20% again, 40%, 60% ethanolic solution gradient elution, flow velocity are 4BV/hr, eluent reclaims ethanol, eluent is concentrated simultaneously, and final drying obtains product: polyphenol content 102% catechin 67% caffeine content 1.03% yield 6.0%.
Example 4
With old green tea 50 grams in Mianyang, Sichuan, with tea=weight ratio lixiviate in 1: 10, water temperature keeps 80 ℃ of lixiviates 40 minutes, through filtrations at different levels and carry dense after, get filtered fluid 200ml, Tea Polyphenols concentration is about 20mg/ml in the tealeaves, pass through 25mm * 300mm nonpolar macroporous adsorption resin with the 4BV/hr flow velocity, Tea Polyphenols and caffeine have 85% to be adsorbed on the resin approximately, obtain the high purification Tea Polyphenols solution of caffeine content with 70% ethanolic solution wash-out again, get this purification Tea Polyphenols solution 100ml by the plain adsorbent post of 25mm * 250mm sugarcane fibre, the operation flow velocity be 4BV/hr when flowing through Tea Polyphenols be adsorbed, caffeine is discharged by flowing through liquid, use 20% again, 40%, 60% ethanolic solution gradient elution, flow velocity are 4BV/hr, eluent reclaims ethanol, eluent is concentrated simultaneously, and final drying obtains product: polyphenol content 101% catechin 60% caffeine content 2% yield 6.0%.
Claims (6)
1. extract the method for Tea Polyphenols from tealeaves, its step is as follows:
1) will pulverize green tea and carry out counter-current extraction, remove tea grounds through mechanical filter;
2) removing tea juice behind the tea grounds successively through the film coarse filtration, the film ultrafiltration, membrane reverse osmosis concentrate carry dense;
3) will carry tea juice after dense with the 1-6BV/hr flow velocity by nonpolar macroporous adsorption resin, with ethanolic solution wash-out from the resin, the Tea Polyphenols solution that obtains purifying;
4) the Tea Polyphenols solution of Ti Chuning by cellulose adsorbent, through the adsorbing and removing caffeine, is used the ethanolic solution gradient elution of 20～90% concentration with the 1-6BV/hr flow velocity again, concentrates to reclaim ethanol, and drying gets the Tea Polyphenols product.
2. the method for extracting Tea Polyphenols from tealeaves according to claim 1 is characterized in that it is 70～90 ℃ that counter-current extraction is pulverized the water temperature of green tea.
3. the method for extracting Tea Polyphenols from tealeaves according to claim 1, the coarse filtration film that it is characterized in that concentrated tea juice are organic polymer or the ceramic pipe type films of removing 10～200,000 Dalton molecular weights.
4. the method for extracting Tea Polyphenols from tealeaves according to claim 1, the milipore filter that it is characterized in that concentrated tea juice are the organic polymer tubular membrane of removing 20,000～100,000 Dalton molecular weights.
5. the method for extracting Tea Polyphenols from tealeaves according to claim 1, the reverse osmosis membrane that it is characterized in that concentrated tea juice are the polysulfones rolling NF membrane that sees through 200 dalton molecules.
6. the method for extracting Tea Polyphenols from tealeaves according to claim 1 is characterized in that said cellulose adsorbent is trees, straw, corncob or bagasse.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101552762A CN100539859C (en) | 2006-12-18 | 2006-12-18 | From tealeaves, extract the method for Tea Polyphenols |
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| CNB2006101552762A CN100539859C (en) | 2006-12-18 | 2006-12-18 | From tealeaves, extract the method for Tea Polyphenols |
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| CN100539859C true CN100539859C (en) | 2009-09-16 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121705B (en) * | 2007-09-21 | 2010-12-08 | 江苏德和生物科技有限公司 | Technique for preparing tea polyphenols |
| CN101461433B (en) * | 2008-11-07 | 2013-06-05 | 健士星生物技术研发(上海)有限公司 | Tea extract and preparation method thereof |
| CN102698070B (en) * | 2011-03-27 | 2013-11-20 | 厦门特伦生物药业有限公司 | Radix astragali-jujube stomach-strengthening tea capsule production process |
| CN102178003A (en) * | 2011-03-30 | 2011-09-14 | 浙江永金茶业有限公司 | Process for extracting tea polyphenol |
| CN112674190A (en) * | 2020-12-24 | 2021-04-20 | 云南省农业科学院茶叶研究所 | Method for extracting low-caffeine, no-pesticide residue and no-ester tea polyphenol from tea leaves |
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2006
- 2006-12-18 CN CNB2006101552762A patent/CN100539859C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 杉树木质纤维素对酯型儿茶素类选择性吸附的研究. 梁慧玲，梁月荣，陆建良，叶俭慧，唐德松.浙江大学学报（农业与生命科学版），第32卷第6期. 2006 |
| 杉树木质纤维素对酯型儿茶素类选择性吸附的研究. 梁慧玲，梁月荣，陆建良，叶俭慧，唐德松.浙江大学学报(农业与生命科学版)，第32卷第6期. 2006 * |
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Application publication date: 20070606 Assignee: Hangzhou Tiancheng Pharmaceutical Co., Ltd. Assignor: Hangzhou Zheda Tea Sci-Tech Co., Ltd. Contract record no.: 2015330000250 Denomination of invention: Supported adsorbent and method for extracting tea polyphenol from tea Granted publication date: 20090916 License type: Exclusive License Record date: 20151105 |
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Assignee: Hangzhou Tiancheng Pharmaceutical Co., Ltd. Assignor: Hangzhou tea Yibao Tea Technology Co., Ltd. Contract record no.: 2015330000250 Date of cancellation: 20181031 |
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Change date: 20181031 Contract record no.: 2015330000250 Assignor after: Hangzhou tea Yibao Tea Technology Co., Ltd. Assignor before: Hangzhou Zheda Tea Sci-Tech Co., Ltd. |
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