CN105712897B - A kind of tea polyphenol extract circulation utilization method - Google Patents
A kind of tea polyphenol extract circulation utilization method Download PDFInfo
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- CN105712897B CN105712897B CN201610049481.4A CN201610049481A CN105712897B CN 105712897 B CN105712897 B CN 105712897B CN 201610049481 A CN201610049481 A CN 201610049481A CN 105712897 B CN105712897 B CN 105712897B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D473/00—Heterocyclic compounds containing purine ring systems
- C07D473/02—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6
- C07D473/04—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms
- C07D473/06—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3
- C07D473/12—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3 with methyl radicals in positions 1, 3, and 7, e.g. caffeine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The present invention relates to a kind of tea polyphenol extract circulation utilization method, including Continuous Countercurrent Extraction：Tea raw material by harvesting, screening pretreatment puts into extraction tank by charging device, is moved in the case where the mechanical force of scraper plate and spiral is promoted along groove, fully contacts after extraction, be discharged after discharging section water squeezing with solvent；Extraction solvent enters after extraction tank, flows from high to low under gravity, and tea extract is discharged from overfall, i.e. catechin slag；Separated using molecular weight 3500Da milipore filter, reverse osmosis membrane and collect the theanine in catechin slag；After the theanine that step is separated is pre-processed by ultrafiltration, decolouring again, it is pH 3.4, liquid concentration 3.0mg/ml, flow velocity 1.7 bed volume per hour to select absorbing process condition, after pH 11.3 ammoniacal liquor elution, obtains theanine；By the catechin slag after the theanine of separation through supercritical CO2Be obtained by extraction caffeine, Tea Polyphenols, it is freeze-dried after obtain product.The Tea Polyphenols purity that this method is obtained is high, and yield is high, is recycled and extracts.
Description
Technical field
The present invention relates to tea polyphenol extract circulation utilization method.
Background technology
Extract Tea Polyphenols effective component yield low, waste big, cost is high；Tea grounds can not be rationally utilized, theanine is discarded；
Take off when washing caffeine without absorption affinity；Nutrient loss.
The content of the invention
In view of the above-mentioned problems, the present invention provides a kind of tea polyphenol extract circulation utilization method, comprise the following steps：
(1) Continuous Countercurrent Extraction：Tea raw material by harvesting, screening pretreatment puts into extraction tank by charging device,
The mechanical force of scraper plate and spiral is moved under promoting along groove, is fully contacted after extraction, is discharged after discharging section water squeezing with solvent；Carry
Take solvent to enter after extraction tank, flow from high to low under gravity, tea extract is discharged from overfall, i.e. catechin
Slag.(2) tea grounds separation tea base acid, is separated using molecular weight 3500Da milipore filter, reverse osmosis membrane and collected in catechin slag
Theanine..Separated using molecular weight 3500Da milipore filter, reverse osmosis membrane and collect the theanine in catechin slag, it is comprehensive
Yield is closed up to 54.05%, product purity is up to 10%, and tea grounds biological value, up to 55%, is the primary raw material of organic fertilizer, so improved
The comprehensive benefit that tealeaves deep development is utilized, reduce further production cost.
(3) ion exchange column technique：Ion-exchange extracts theanine；The theanine that step (2) is separated is again by super
After filter, pretreatment of decolourizing, it is pH 3.4, liquid concentration 3.0mg/ml, flow velocity 1.7 post bed body per hour to select absorbing process condition
Product, after pH 11.3 ammoniacal liquor elution, obtains theanine.It is 58% to obtain theanine content, and the theanine rate of recovery is 82%,
While benefit is obtained, contaminated wastewater is decreased
(4) supercritical CO2Extraction process：Catechin slag after the theanine that step (2) is separated is through supercritical CO2Extraction
Obtain caffeine, Tea Polyphenols, it is freeze-dried after obtain product.
Solvent in step (1) is any one in water, ethanol, acetone, preferably water.
In step (1), both tea raw material and solvent do reverse extraction, and the contact surface of tea raw material and solvent is in all the time
Under concentration difference state, by multistage vadose solution extraction after, tealeaves material residue is discharged, and extract solution then by effective content of tea step by step
Penetrate into and become high concentration extract solution, and flowed out from opposite direction.
The mass concentration difference of the contact surface of tea raw material and solvent is 20%-30%, and extract solution is then by effective content of tea
Penetrate into step by step and become high concentration extract solution, the mass concentration of its high concentration extract solution is 70%-80%.
Means of supercritical extraction described in step (4) can also be extracted for algae, i.e. after the theanine for separating step (2)
Catechin slag is placed in algae, in dark, after stirring 10-12h, is used ethanol solution gradient elution, is reclaimed ethanol fluidised bed spraying
Tea Polyphenols is can obtain after drying.
Described algae is any one in chlorella, Nannochloropsis oculata, very thin Euglena, spirulina maxim.Described youngster
Theine slag and the mass ratio of algae are 10-15：1-3.
Algae has stronger absorption property, and the present invention is using algae by the Tea Polyphenols in catechin slag in dark (illumination
The growth of chlorella can be influenceed) under the conditions of adsorbed, it is to be adsorbed after the completion of, then in ethanol solution elution be adsorbed with Tea Polyphenols
Algae, make Tea Polyphenols purer.
In the present invention, Continuous Countercurrent Extraction, the technique is applied to during tea comprehensive processing, and tealeaves and hot water are extracting dress
While making the continuous flow upstream motion of opposite direction in putting, realize that the continuous isolation of tea juice or extract is made in counter-current process
Industry, tealeaves inclusion leaching rate is high.Compared with the domestic intermittent extraction process generally used at present, Continuous Countercurrent Extraction has
The advantage that extract concentration is high, effective component extraction rate is high, can improve tea raw material utilization rate.
The technique realizes that the totally-enclosed operation of serialization, dynamic countercurrent are extracted, and plays saving manpower, reduces solvent load, drop
Low production cost, the effect for improving production efficiency.By charging device, transportation sprocket component, transmission belt, scraper plate, solvent inlet, carry
Liquid outlet, slag-drip opening etc. is taken to constitute.First, the tea raw material by pretreatment puts into extraction tank by charging device, in scraper plate and
The mechanical force of spiral is moved under promoting along groove, is fully contacted after extraction, is discharged after discharging section water squeezing with water equal solvent；Water etc.
Extraction solvent enters after extraction tank, flows from high to low under gravity, and tea extract is discharged from overfall.Tea raw material
With the Extraction solvent such as water, both make reverse movement, and contact interface is under concentration difference state all the time, is extracted by multistage vadose solution
Afterwards, tealeaves material residue is discharged, and extract solution then becomes high concentration extract solution due to the infiltration step by step of effective content of tea, slave phase
Anti- direction outflow, so as to realize the extraction to greatest extent of active ingredient in tealeaves.
Supercritical CO2In extraction process, CO2It is nonpolar molecule, caffeine is also nonpolar molecule, and catechin is pole
Property molecule, so caffeine is easily by supercritical CO2Extraction, and Tea Polyphenols is in supercritical CO2Middle dissolution rate is extremely low, thus can be used for
Extract caffeine, purifying Tea Polyphenols.Supercritical fluid be in critical-temperature, more than critical pressure, between gas and liquid it
Between fluid.Supercritical fluid extraction, is exactly using a certain critical fluids (the such as CO as solvent2) mixed with solid or liquid
Thing is contacted, and using balancing each other and transmission characteristic for their "abnormal", extracts object, then using the side of decompression or heating
Method, reduces the density (dissolving power) of extraction phase, then solvent is separated with extract, is balanced each other shape using each component under different condition
The difference of state is separated.Compared with other extracting process, supercritical fluid extraction has that rate of extraction is fast, consumed energy is few, molten
Agent consumption is few, the advantages of do not remain.In the extraction of thermographic compound, can make to be extracted material not because oxidation, decompose,
Loss and go bad.Can have much as the material of supercritical fluid, wherein with CO2 better performances, 1) it is inexpensive, high-purity gas is easily made
Body.2) critical-temperature is low, be easy to operation, be adapted to heat-sensitive substance extract it is 3) nontoxic, tasteless, do not remain, it is nonflammable, do not pollute ring
Border.4) chemical inertness, it is to avoid Tea Polyphenols is aoxidized.
The present invention is also using lignocellulosic adsorption column separation.Lignin and cellulose, hemicellulose are strings
Main component.Using waste materials such as wood chips, in the material by the processing of soda acid, lignin is deposited simultaneously with cellulose
In referred to as lignocellulosic.The material has good adsorption effect to Polyphenols in solution, but to caffeine without energy of adsorption
Power.Tea Polyphenols solution is removed into caffeine through lignocellulosic post, ethanol solution gradient elution is used, ethanol, fluid bed spray is reclaimed
Mist obtains polyphenol content after drying>98%th, catechin total amount 60-95%, EGCG content 60%-90%, caffeine content
0.5%-1%.Yield 10%-11%.
Vacuum freeze drying, also known as vacuum freeze-drying, molecule are dried.Carried applied to the tealeaves with high added value
The processing of thing is taken, its operation principle is to freeze tea extract for -35 DEG C now, moisture is changed into solid ice, then higher
Vacuum under, ice is directly distilled and removed for gaseous form, material dewatering is dried.The drying process of low temperature, vacuum, most
The color for maintaining dried object of limits, shape, and protect contained nutritional ingredient.
Continuous Countercurrent Extraction has extract concentration height, effective component extraction rate high；
Separated using molecular weight 3500Da milipore filter, reverse osmosis membrane and improve the comprehensive effect that tealeaves deep development is utilized
Benefit, reduce further production cost；
Ion-exchange extracts theanine, and it is 58% to obtain theanine content, and the theanine rate of recovery is 82%, is being imitated
While beneficial, contaminated wastewater is decreased；
Supercritical fluid extraction has that rate of extraction is fast, consumed energy is few, solvent-oil ratio is few, do not remain.
Embodiment
Embodiment 1
A kind of tea polyphenol extract circulation utilization method, comprises the following steps：
(1) Continuous Countercurrent Extraction：Tea raw material by harvesting, screening pretreatment puts into extraction tank by charging device,
The mechanical force of scraper plate and spiral is moved under promoting along groove, is fully contacted after extraction, is discharged after discharging section water squeezing with water；Extract
Solvent enters after extraction tank, flows from high to low under gravity, and tea extract is discharged from overfall, i.e. catechin slag；
Both tea raw material and solvent do reverse extraction, and the contact surface of tea raw material and solvent is in concentration difference shape all the time
Under state, after the extraction of multistage vadose solution, tealeaves material residue is discharged, and extract solution is then penetrated into and become step by step by effective content of tea
High concentration extract solution, and flowed out from opposite direction.The mass concentration difference of the contact surface of tea raw material and solvent is 25%, is extracted
Liquid is then penetrated into and becomes high concentration extract solution step by step by effective content of tea, and the mass concentration of its high concentration extract solution is 74%.
(2) tea grounds separation tea base acid, is separated using molecular weight 3500Da milipore filter, reverse osmosis membrane and collects the tea in catechin slag
Propylhomoserin；
(3) ion exchange column technique：Ion-exchange extracts theanine；
After the theanine that step (2) is separated is pre-processed by ultrafiltration, decolouring again, it is pH to select absorbing process condition
3.4th, liquid concentration 3.0mg/ml, flow velocity 1.7 bed volume per hour, after pH 11.3 ammoniacal liquor elution, obtains theanine；
(4) supercritical CO2Extraction process：Catechin slag after the theanine that step (2) is separated is through supercritical CO2Extraction
Obtain caffeine, Tea Polyphenols, it is freeze-dried after obtain product.
Obtained theanine content is 58%, and the theanine rate of recovery is 82%, polyphenol content ＞ 99%, catechin total amount
For 81%, EGCG content is 79.3%, and caffeine content is 0.74%.
Embodiment 2
A kind of tea polyphenol extract circulation utilization method, comprises the following steps：
(1) Continuous Countercurrent Extraction：Tea raw material by harvesting, screening pretreatment puts into extraction tank by charging device,
The mechanical force of scraper plate and spiral is moved under promoting along groove, is fully contacted after extraction, is discharged after discharging section water squeezing with water；Extract
Solvent enters after extraction tank, flows from high to low under gravity, and tea extract is discharged from overfall, i.e. catechin slag；
Both tea raw material and solvent do reverse extraction, and the contact surface of tea raw material and solvent is under concentration difference state all the time, warp
Cross after multistage vadose solution extraction, tealeaves material residue is discharged, and extract solution is then penetrated into and becomes high concentration step by step by effective content of tea
Extract solution, and being flowed out from opposite direction, the mass concentration difference of the contact surface of tea raw material and solvent is 22%, extract solution then by
Effective content of tea penetrates into and becomes high concentration extract solution step by step, and the mass concentration of its high concentration extract solution is 80%.(2) tea grounds
Tea base acid is separated, is separated using molecular weight 3500Da milipore filter, reverse osmosis membrane and collects the theanine in catechin slag；
(3) ion exchange column technique：Ion-exchange extracts theanine；
After the theanine that step (2) is separated is pre-processed by ultrafiltration, decolouring again, it is pH to select absorbing process condition
3.4th, liquid concentration 3.0mg/ml, flow velocity 1.7 bed volume per hour, after pH 11.3 ammoniacal liquor elution, obtains theanine；
(4) the catechin slag after the theanine for separating step (2) is placed in chlorella (described catechin slag and algae
Mass ratio be 10：1) in dark, after stirring 10-12h, ethanol solution gradient elution is used, ethanol fluidised bed spray drying is reclaimed
It can obtain Tea Polyphenols afterwards.
Obtained theanine content is 58%, and the theanine rate of recovery is 82%, polyphenol content ＞ 99%, catechin total amount
For 96%, EGCG content is 85%, and caffeine content is 0.88%.
Embodiment 3
Step leads to embodiment 2, enters chlorella and replaces with Nannochloropsis oculata, and the mass ratio of catechin slag and algae is 12：1.6.
Obtained theanine content is 58%, and the theanine rate of recovery is 82%, polyphenol content ＞ 99%, and catechin total amount is
94.5%, EGCG content is 83.2%, and caffeine content is 0.7%.
Embodiment 4
Step leads to embodiment 2, enters chlorella and replaces with very thin Euglena, and the mass ratio of catechin slag and algae is 13：2.2.
Obtained theanine content is 58%, and the theanine rate of recovery is 82%, polyphenol content ＞ 99%, and catechin total amount is
91.9%, EGCG content is 86.7%, and caffeine content is 0.65%.
Embodiment 4
Step leads to embodiment 2, enters chlorella and replaces with spirulina maxim, and the mass ratio of catechin slag and algae is 14：3.
Obtained theanine content is 58%, and the theanine rate of recovery is 82%, polyphenol content ＞ 99%, and catechin total amount is
95.5%, EGCG content is 82.6%, and caffeine content is 0.72%.
Claims (5)
1. a kind of tea polyphenol extract circulation utilization method, it is characterised in that comprise the following steps：
（1）Continuous Countercurrent Extraction：Tea raw material by harvesting, screening pretreatment puts into extraction tank by charging device, in scraper plate
And moved under the mechanical force promotion of spiral along groove, fully contact after extraction, be discharged after discharging section water squeezing with solvent；Extract molten
Agent enters after extraction tank, flows from high to low under gravity, and tea extract is discharged from overfall, i.e. catechin slag；
（2）Tea grounds separation tea base acid, is separated using molecular weight 3500Da milipore filter, reverse osmosis membrane and collects catechin slag
In theanine；
（3）Ion exchange column technique：Ion-exchange extracts theanine；By step（2）The theanine of separation is again by ultrafiltration, de-
After color pretreatment, it is pH 3.4, liquid concentration 3.0mg/ml, flow velocity 1.7 bed volume per hour to select absorbing process condition,
After pH 11.3 ammoniacal liquor elution, theanine is obtained；
（4）Algae extraction process：By step（2）Catechin slag after the theanine of separation is placed in algae, in dark, stirring
After 10-12h, ethanol solution gradient elution is used, reclaims and can obtain Tea Polyphenols, described algae after ethanol fluidised bed spray drying
Class is any one in chlorella, Nannochloropsis oculata, very thin Euglena, spirulina maxim, described catechin slag and the matter of algae
Amount is than being 10-15：1-3.
2. the tea polyphenol extract circulation utilization method described in claim 1, it is characterised in that step（1）In solvent be
Any one in water, ethanol, acetone.
3. the tea polyphenol extract circulation utilization method described in claim 1, it is characterised in that step（1）In solvent be
Water.
4. the tea polyphenol extract circulation utilization method described in claim 1, it is characterised in that step（1）In, tea raw material
Reverse extraction is done with both solvents, and the contact surface of tea raw material and solvent is under concentration difference state all the time, is oozed by multistage
After molten extraction, tealeaves material residue is discharged, and extract solution is then penetrated into and becomes high concentration extract solution step by step by effective content of tea, and
Flowed out from opposite direction.
5. the tea polyphenol extract circulation utilization method described in claim 1, it is characterised in that tea raw material and solvent connect
The mass concentration difference of contacting surface is 20%-30%, and extract solution is then penetrated into and becomes high concentration extract solution step by step by effective content of tea,
The mass concentration of its high concentration extract solution is 70%-80%.
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| CN107712169B (en) * | 2017-11-20 | 2021-05-25 | 福建省农业科学院茶叶研究所 | Tea processing method |
| CN107913530A (en) * | 2017-11-24 | 2018-04-17 | 广西中港高科国宝金花茶产业有限公司 | A kind of CO2The method that supercritical methanol technology fluid extracts tea polyphenols from Camellia nitidissima |
| CN110437203B (en) * | 2019-07-15 | 2022-05-27 | 湖南鑫文天生物科技有限公司 | Large-scale continuous countercurrent extraction and supercritical carbon dioxide extraction nicotine combined process |
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| CN1557841A (en) * | 2004-01-14 | 2004-12-29 | 中国农业科学院茶叶研究所 | Process for synthetic extraction of polysaccharides, tea-polyphenol, theanine, caffeine from tea |
| CN100404523C (en) * | 2006-02-21 | 2008-07-23 | 张守政 | Process for extracting tea polyphenol, theanine, tea polysaccharide and tea pigment from tea |
| 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 |
| CN103242314B (en) * | 2013-04-19 | 2015-06-24 | 天津大学 | Method for comprehensively extracting effective ingredients in tea |
| CN103992359A (en) * | 2014-05-08 | 2014-08-20 | 梁树钦 | Preparation process for extracting green tea polyphenols from tea |
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