CN109535119A - A kind of extracting method of tea polyphenols - Google Patents
A kind of extracting method of tea polyphenols Download PDFInfo
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- CN109535119A CN109535119A CN201811611841.0A CN201811611841A CN109535119A CN 109535119 A CN109535119 A CN 109535119A CN 201811611841 A CN201811611841 A CN 201811611841A CN 109535119 A CN109535119 A CN 109535119A
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- tea polyphenols
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- 241001122767 Theaceae Species 0.000 title claims abstract description 70
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 53
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 70
- 239000000284 extract Substances 0.000 claims abstract description 25
- 230000001376 precipitating effect Effects 0.000 claims abstract description 18
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000000428 dust Substances 0.000 claims description 17
- 239000003153 chemical reaction reagent Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 239000013049 sediment Substances 0.000 claims description 11
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical group [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 11
- 229960001763 zinc sulfate Drugs 0.000 claims description 11
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 11
- 239000000287 crude extract Substances 0.000 claims description 10
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 9
- 235000002906 tartaric acid Nutrition 0.000 claims description 9
- 239000011975 tartaric acid Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 239000012044 organic layer Substances 0.000 claims description 6
- 239000012074 organic phase Substances 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 6
- 238000004853 microextraction Methods 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M sodium bicarbonate Substances [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000000967 suction filtration Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 description 13
- 238000005516 engineering process Methods 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000000926 separation method Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000010992 reflux Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 206010028980 Neoplasm Diseases 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- UGAPHEBNTGUMBB-UHFFFAOYSA-N acetic acid;ethyl acetate Chemical compound CC(O)=O.CCOC(C)=O UGAPHEBNTGUMBB-UHFFFAOYSA-N 0.000 description 2
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 2
- 229960001948 caffeine Drugs 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002024 ethyl acetate extract Substances 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 description 2
- 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 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 208000008589 Obesity Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
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- 230000000840 anti-viral effect Effects 0.000 description 1
- 230000002155 anti-virotic effect Effects 0.000 description 1
- 239000003472 antidiabetic agent Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 1
- 235000005487 catechin Nutrition 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 229950001002 cianidanol Drugs 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
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- 239000003337 fertilizer Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229940074391 gallic acid Drugs 0.000 description 1
- 235000004515 gallic acid Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000010262 high-speed countercurrent chromatography Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
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- 210000000214 mouth Anatomy 0.000 description 1
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- 229930014626 natural product Natural products 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 235000020824 obesity Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000000049 pigment Substances 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
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Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to tea polyphenol extract technical fields, especially a kind of extracting method of tea polyphenols, present invention process is including impregnating, extracting, be centrifuged, precipitating suction filtration, turn molten and six steps of extraction, pass through the adjustment to each process parameter, largely retain effective component, improve added value of product, and recovery rate that is effective and improving tea polyphenols, reduce impurity content, improve the quality of product, it is coupled in particular by homogenate extraction technology and micro-control abstraction technique, has the characteristics that efficient, quick, low energy consumption, environmentally friendly, controllability is strong.
Description
Technical field
The present invention relates to tea polyphenol extract technical field, especially a kind of extracting method of tea polyphenols.
Background technique
With the development of science and technology, the extraction separation of active ingredient of natural product obtains fabulous development with application,
It is deeply constantly found with the new function of tea polyphenols with research again, people are growing day by day to the interest of tea polyphenols, tea polyphenols
It is not only a kind of natural nontoxic antioxidant, and is also a kind of ideal natural drug, has and removes free radical and antioxygen
Change etc. bioactivity, antibacterial, antiviral, cancer-resisting, inhibit tumour, in terms of have good function
Effect, the production and selling of tea polyphenols at home and abroad have more than ten years history, and tea polyphenols product is mainly used for tumour medicine, the heart at present
Vascular health drug, anti-diabetic and obesity health medicine, anti-virus formulation, cosmetics, food oxydating resistance additive, oral cavity
Clean-preserving agent, beverage freshness remaining agent, color preserving agent, deodorant etc..
World's tea yield in 2001 is up to 302.2 ten thousand tons, and the total volume of exports is up to 138.86 ten thousand tons, with each Tea Production state tea
The sustainable growth of leaf-making quantity, contradiction becomes increasingly conspicuous between tealeaves production-supply-marketing, and Tea Production benefit constantly declines, and tealeaves was producing
A large amount of tea grounds, the tea dust generated in journey generally utilizes directly as soil and fertilizer, causes the waste of resource, to promote economy
Development, deep processing, comprehensive utilization and the effective content of tea of tealeaves extract aspect and are flourished, especially mentioned from tea dust
The technology for taking tea polyphenols, in China also in the elementary step, most of technology all also rests on experimental stage, it is difficult to realize industry
Metaplasia produces.
Traditional traditional extraction is uniformly to stand extractant and material liquid afterwards in separatory funnel, is then existed using substance
Solubility or the difference of distribution coefficient, a kind of method for making solute substance be transferred to another solvent from solvent in two kinds of solvents；
This method is not only cumbersome bothersome, is also consumed by a large amount of solvents, and certain toxic solvents can also damage human body；In recent years, it closes
Unprecedented development has also been obtained in the extraction separation of tea polyphenols, purification technique, other than Conventional processing methods, and has been occurred newly
Extraction and separation technology, such as supercritical extraction, high-speed countercurrent chromatography conclude these extraction separation and purification technologies
It summarizes, is broadly divided into two steps mostly, first is that extracting the thick tea polyphenols containing caffeine from tea dust, second is that by separation concentration, mentioning
The tea polyphenols of pure obtained high-purity, and these prior arts, generally based on solvent, the solvent mainly taken has water, first
Alcohol, ethyl alcohol, acetone, ethyl acetate etc., the then method for removing impurity mainly have go out caffeine, active carbon and petroleum ether of chloroform de-
Pigment, chlorophyll and polysaccharide etc., then used the precipitation method, solvent extraction, chromatography etc. and realize purification process, and by extraction
The mode taken makes tea polyphenols be extracted out from above-mentioned solvent.
As it can be seen that at present process for extracting tea polyphenol also it is continuous improve and heuristic process in, have the defects that it is more, such as
Supercritical extraction, input cost during the extraction process is higher, inconvenient for operation, and largely uses organic solvent, makes to obtain
A large amount of poisonous and hazardous ingredients and heavy metal ion are remained in the tea polyphenols obtained, to also reduce the product of tea polyphenols product
Matter；And use and be heated to reflux, the methods of ultrasonic extraction is longer there are extraction time, energy consumption is higher；For another example " homogenate extraction is green for document
The technical study of tea polyphenols in tea ", Zhu Xingyi；Yang Junhui；Xie Jie etc., the technique for having studied homogenate extraction Tea Polyphenols,
Single factor exploration is carried out to concentration of alcohol, solid-liquid ratio, extraction time and extraction time, carries out orthogonal experiment plan according to result is investigated
Meter, then carries out verification test, and the process conditions are compared with traditional heating refluxing extraction mode；The result shows that most
Good extracting factor are as follows: concentration of alcohol 60%, solid-liquid ratio 1g: 20mL, homogenate extraction time 40s are extracted 2 times, and tea polyphenols obtain
Rate 18.22%；Compared with conventional solvent circumfluence method, homogenate extraction method yield improves 1.76 percentage points, and ethanol consumption is reduced
46.7%, extraction time greatly shortens, but its recovery rate is undesirable, and purity is not high.
Based on this, the present invention on the basis of existing technology, is improved by the processing step to tea polyphenol extract, and
The solvent and other reagents selected in the extraction process of tea polyphenols are comprehensively considered, is extracted with short flash and micro-control extracts two
Person combines, and provides a kind of new approaches for the novel technology for extracting of tea polyphenols.
Summary of the invention
In order to solve the above technical problems existing in the prior art, the present invention provides a kind of extraction sides of tea polyphenols
Method, comprising the following steps:
(1) it impregnates: tea dust being impregnated using water, the additional amount of water is 20-30 times of tea dust weight, when immersion
Between be 45-75min；
(2) it extracts: above-mentioned material being put into flash extracter and is extracted, extractions voltage is 100-220V, and extraction time is
60-120s obtains crude extract；
(3) be centrifuged: by above-mentioned crude extract with supercentrifuge be centrifuged 5-15min, revolving speed 3000-4000r/min, obtain from
Heart liquid；
(4) precipitating filters: precipitating reagent being added into centrifugate and is precipitated, and uses NaHCO3PH value 5.5-6.5 is adjusted,
It filters, obtains sediment；
(5) turn molten: 1-10% tartaric acid being added into sediment and carries out turning molten, molten object must be turned；
(6) it extracting: molten object will be turned and be sent into micro-extraction equipment, use ethyl acetate for extractant, micro-control extracts 1-3 times,
Obtained extract liquor is stood to complete layering, to get tea polyphenols after taking organic layer to be concentrated and dried.
The temperature of above-mentioned water is 50-90 DEG C.
It is 100V, extraction time 90s that above-mentioned steps (2), which extract voltage,.
Above-mentioned precipitating reagent is zinc sulfate.
Above-mentioned food level zinc sulfate adds 0.5-1g according to every mL centrifugate.
Water phase in above-mentioned micro-control extraction process: organic phase=3:1, extraction time 15-30min.
Above-mentioned zinc sulfate, tartaric acid are food-grade.
Beneficial effect
1. the present invention uses homogenate extraction, effective to shorten extraction time, solvent usage is reduced, under normal temperature conditions energy
It realizes the coarse extraction to tealeaves and tea dust, effectively protects the oxidizable ingredient of thermal sensitivity in tealeaves and tea dust, improve and produce
The added value of product is foreshortened to 1-2 minutes compared to traditional extraction process by original a few hours extracting cycle, significant to improve
Working effect, simplifies operation；
2. micro-control extraction of the present invention is that extractant and material liquid are passed through in the reaction channel of microreactor, mixing extraction is carried out
It takes, since the micro-structure inside microreactor makes microreactor equipment have great specific surface area, in constant-flux pump extraction
After agent and raw material liquid pump such as microreactor, solvent can sufficiently be mixed in the pipeline inside microreactor with extracting solution
It closes, is dissolved in the effective component of extracting solution among solvent, to complete hybrid extraction work, improve extraction efficiency.Microchannel plate
The application for answering device plays an important role for solving the problems, such as safety and environmental protection and resource consumption serious problems.
3. present invention selection food-grade reagent, and then avoid the risk of metal ion, soda acid pollution；The present invention is using sudden strain of a muscle
Formula extractive technique and the coupling of micro-control abstraction technique have the characteristics that efficient, quick, low energy consumption, environmentally friendly, controllability is strong, and gained mentions
Take liquid and extract liquor color clearly demarcated, no emulsion occurs, and present invention process technology is novel, easy to industrialized production.
4. the present invention is coupled using homogenate extraction technology and micro-control abstraction technique, tea dust is made full use of to realize tea polyphenols
Extraction, to reach the utilization rate to useless tealeaves, this method is equally applicable to the extraction separation of the plant containing tea polyphenols,
It is easy to industrialized production.
5. present invention process is including impregnating, extracting, centrifugation, precipitating suction filtration, turns molten and six steps of extraction, by each step
The adjustment of rapid technological parameter, largely retains effective component, improves added value of product, and effectively improve tea polyphenols
Recovery rate, reduce impurity content, improve the quality of product.
Extracting mode research: using tea dust as raw material, homogenate extraction, heating and refluxing extraction, ultrasonic wave extraction etc. three is selected
The different extracting mode of kind, investigates its influence to tea polyphenol extract rate；According to GB/T8313-2008 " Tea Polyphenols in Tea and
The detection method of catechin content " content of tea polyphenols in each extracting solution of measurement, as a result such as the following table 1:
The absorbance of comparative sample and standard working solution, calculation formula are as follows:
A- sample test liquid absorbance；V- sample extracting solution volume；D- dilution gfactor (usually 1mL is diluted to 100mL,
Then 100) its dilution gfactor is；SLOPEStdThe slope of gallic acid standard curve；M- sample dry matter content %；m1Sample
Quality, unit g；Standard curve is shown in attached drawing Fig. 1；
Table 1
By test result in table 1 it is found that being mentioned using homogenate extraction polyphenol content higher than heating and refluxing extraction and ultrasonic wave
It takes, the time is also greatly saved, overall merit homogenate extraction is better than refluxing extraction and ultrasonic wave extraction.
Extraction/way of purification research: using ethyl acetate as extractant, the extraction that above-mentioned homogenate extraction obtains is extracted
Tea polyphenols, the extraction of micro-control extraction and traditional extraction mode more of the present invention is made in liquid, the concentrated drying of obtained upper organic phase
Effect is taken, as a result such as the following table 2
Table 2
As it can be seen that traditional technology extracting process is below micro-control extraction process as a result, and micro-control technology is traditional technology
1.37 times (HCL), 1.39 times (tartaric acid), so the product yield obtained using extracting process of the present invention is higher.
The tea polyphenols filtrate of the winestone acid dissolution of 0.4mol/L HCL and 5% is used respectively, after being extracted with ethyl acetate, as evidence
Bright tartaric acid can replace dissolving with hydrochloric acid precipitating, by the organic layer being obtained by extraction be respectively adopted HPLC detection contained substance whether one
Sample, chromatographic column be Agilent ZORBAX SB-C18,5 μm, 4.6 × 250m；Chromatographic condition is mobile phase (methanol: N, N- dimethyl
Formamide: 1% acetic acid) 10:15:75,30 DEG C of column temperature, Detection wavelength 280nm, the two obtained material is proved by gained chromatogram
Identical and tea polyphenols standard sample is identical, then proves that sediment can be dissolved with winestone acid instead of HCl to reduce soda acid pollution；
Specifically it is detailed in Fig. 2, Fig. 3 and Fig. 4.
Detailed description of the invention
Fig. 1 is the canonical plotting of polyphenol content measurement；
Fig. 2 is tea polyphenols standard sample chromatogram；
Acetic acid ethyl acetate extract chromatogram after Fig. 3 is dissolved by 0.4mol/L HCL；
Acetic acid ethyl acetate extract chromatogram after Fig. 4 is dissolved by 5% tartaric acid；
Specific embodiment
Tuberculosis specific embodiment is limited technical solution of the present invention is further below, but claimed
Range is not only limited to made description.
Embodiment 1
A kind of extracting method of tea polyphenols, comprising the following steps:
(1) it impregnates: tea dust being impregnated using water, the additional amount of water is 20 times of tea dust weight, soaking time
For 45min；
(2) extract: above-mentioned material is put into flash extracter and is extracted, extractions voltage be 100V, extraction time 60s,
Obtain crude extract；
(3) it is centrifuged: above-mentioned crude extract supercentrifuge being centrifuged 5min, revolving speed 3000r/min obtains centrifugate
1035ml；
(4) precipitating filters: precipitating reagent being added into centrifugate and is precipitated, and uses NaHCO3PH value 5.5 is adjusted, is taken out
Filter, obtains sediment；
(5) turn molten: 4% tartaric acid being added into sediment and carries out turning molten, molten object must be turned；
(6) it extracts: molten object will be turned and be sent into micro-extraction equipment, use ethyl acetate for extractant, micro-control extracts 1 time, obtains
To extract liquor stand to complete layering and obtain tea polyphenols 0.516g after taking organic layer to be concentrated and dried.
The temperature of above-mentioned water is 60 DEG C.
Above-mentioned precipitating reagent is zinc sulfate.
Above-mentioned food level zinc sulfate adds 0.5g according to every mL centrifugate.
Water phase in above-mentioned micro-control extraction process: organic phase=3:1, extraction time 15min.
Embodiment 2
A kind of extracting method of tea polyphenols, comprising the following steps:
(1) it impregnates: tea dust being impregnated using water, the additional amount of water is 30 times of tea dust weight, soaking time
For 75min；
(2) extract: above-mentioned material is put into flash extracter and is extracted, extractions voltage be 100V, extraction time 120s,
Obtain crude extract；
(3) it is centrifuged: above-mentioned crude extract supercentrifuge being centrifuged 15min, revolving speed 4000r/min obtains centrifugate
1025ml；
(4) precipitating filters: precipitating reagent being added into centrifugate and is precipitated, and uses NaHCO3PH value 6.5 is adjusted, is taken out
Filter, obtains sediment；
(5) turn molten: 6% tartaric acid being added into sediment and carries out turning molten, molten object must be turned；
(6) it extracts: molten object will be turned and be sent into micro-extraction equipment, use ethyl acetate for extractant, micro-control extracts 3 times, obtains
To extract liquor stand to complete layering and obtain tea polyphenols 0.502g after taking organic layer to be concentrated and dried.
The temperature of above-mentioned water is 70 DEG C.
Above-mentioned precipitating reagent is zinc sulfate.
Above-mentioned food level zinc sulfate adds 1g according to every mL centrifugate.
Water phase in above-mentioned micro-control extraction process: organic phase=3:1, extraction time 25min.
Embodiment 3
A kind of extracting method of tea polyphenols, comprising the following steps:
(1) it impregnates: tea dust being impregnated using water, the additional amount of water is 20 times of tea dust weight, soaking time
For 60min；
(2) extract: above-mentioned material is put into flash extracter and is extracted, extractions voltage be 100V, extraction time 90s,
Obtain crude extract；
(3) it is centrifuged: above-mentioned crude extract supercentrifuge being centrifuged 15min, revolving speed 3500r/min obtains centrifugate
1010.5ml；
(4) precipitating filters: precipitating reagent being added into centrifugate and is precipitated, and uses NaHCO3PH value 6 is adjusted, is filtered,
Obtain sediment；
(5) turn molten: 5% tartaric acid being added into sediment and carries out turning molten, molten object must be turned；
(6) it extracts: molten object will be turned and be sent into micro-extraction equipment, use ethyl acetate for extractant, micro-control extracts 3 times, obtains
To extract liquor stand to complete layering and obtain tea polyphenols 0.535g after taking organic layer to be concentrated and dried.
The temperature of above-mentioned water is 65 DEG C.
Above-mentioned precipitating reagent is zinc sulfate.
Above-mentioned food level zinc sulfate adds 0.8g according to every mL centrifugate.
Water phase in above-mentioned micro-control extraction process: organic phase=3:1, extraction time 20min.
It is important to point out that, above embodiments and test example are only limitted to do further technical solution of the present invention herein
Elaboration and understanding, should not be understood as it is further to technical solution of the present invention limited, what those skilled in the art made
The innovation and creation of non-protruding essential characteristics and marked improvement still fall within protection category of the invention.
Claims (6)
1. a kind of extracting method of tea polyphenols, which comprises the following steps:
(1) it impregnates: tea dust being impregnated using water, the additional amount of water is 20-30 times of tea dust weight, and soaking time is
45-75min；
(2) it extracts: above-mentioned material being put into flash extracter and is extracted, extraction voltage is 100-220V, extraction time 60-
120s obtains crude extract；
(3) it is centrifuged: above-mentioned crude extract supercentrifuge being centrifuged 5-15min, revolving speed 3000-4000r/min must be centrifuged
Liquid；
(4) precipitating filters: precipitating reagent being added into centrifugate and is precipitated, and uses NaHCO3PH value 5.5-6.5 is adjusted, is filtered,
Obtain sediment；
(5) turn molten: 1-10% tartaric acid being added into sediment and carries out turning molten, molten object must be turned；
(6) it extracts: molten object will be turned and be sent into micro-extraction equipment, use ethyl acetate for extractant, micro-control extracts 1-3 times, obtains
Extract liquor stand to complete layering, to get tea polyphenols after taking organic layer to be concentrated and dried.
2. the extracting method of tea polyphenols as described in claim 1, which is characterized in that the temperature of the water is 50-90 DEG C.
3. the extracting method of tea polyphenols as described in claim 1, which is characterized in that it is 100V that the step (2), which extracts voltage, is mentioned
Taking the time is 90s.
4. the extracting method of tea polyphenols as described in claim 1, which is characterized in that the precipitating reagent is zinc sulfate.
5. the extracting method of tea polyphenols as described in right will go 4, which is characterized in that the food level zinc sulfate is centrifuged according to every mL
Liquid adds 0.5-1g.
6. the extracting method of tea polyphenols as described in claim 1, which is characterized in that water phase in the micro-control extraction process: organic
Phase=3:1, extraction time 15-30min.
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| CN111297977A (en) * | 2020-02-12 | 2020-06-19 | 佛山市鼎科科技发展有限公司 | Tea polyphenol extraction method based on complex precipitation |
| CN112858604A (en) * | 2021-01-06 | 2021-05-28 | 华润怡宝饮料（中国）有限公司 | Evaluation method of tea extraction end point |
| CN113884605A (en) * | 2021-10-14 | 2022-01-04 | 安徽科技学院 | Grading type efficient separation and purification method for soil phenolic substances |
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