CN112245506A - Tea polyphenol extraction method - Google Patents
Tea polyphenol extraction method Download PDFInfo
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- CN112245506A CN112245506A CN202011353114.6A CN202011353114A CN112245506A CN 112245506 A CN112245506 A CN 112245506A CN 202011353114 A CN202011353114 A CN 202011353114A CN 112245506 A CN112245506 A CN 112245506A
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- tea polyphenol
- tea
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- polyphenol
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- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 75
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 75
- 238000000605 extraction Methods 0.000 title claims abstract description 21
- 241001122767 Theaceae Species 0.000 claims abstract description 95
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012266 salt solution Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 12
- 239000000287 crude extract Substances 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 11
- 239000003480 eluent Substances 0.000 claims abstract description 10
- 239000011347 resin Substances 0.000 claims abstract description 10
- 229920005989 resin Polymers 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 238000001179 sorption measurement Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000000284 extract Substances 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 21
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 20
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 12
- 235000011164 potassium chloride Nutrition 0.000 claims description 8
- 239000001103 potassium chloride Substances 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 238000009832 plasma treatment Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract 1
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 8
- 230000002829 reductive effect Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 6
- 229960001948 caffeine Drugs 0.000 description 6
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 6
- 230000009471 action Effects 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- -1 superoxide ion Chemical class 0.000 description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 235000013361 beverage Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- XMOCLSLCDHWDHP-IUODEOHRSA-N epi-Gallocatechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@H]2O)=CC(O)=C(O)C(O)=C1 XMOCLSLCDHWDHP-IUODEOHRSA-N 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 150000003254 radicals Chemical group 0.000 description 2
- PFTAWBLQPZVEMU-ZFWWWQNUSA-N (+)-epicatechin Natural products C1([C@@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-ZFWWWQNUSA-N 0.000 description 1
- PFTAWBLQPZVEMU-UKRRQHHQSA-N (-)-epicatechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-UKRRQHHQSA-N 0.000 description 1
- 201000001320 Atherosclerosis Diseases 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 108010078851 HIV Reverse Transcriptase Proteins 0.000 description 1
- XMOCLSLCDHWDHP-UHFFFAOYSA-N L-Epigallocatechin Natural products OC1CC2=C(O)C=C(O)C=C2OC1C1=CC(O)=C(O)C(O)=C1 XMOCLSLCDHWDHP-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000003471 anti-radiation Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 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
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001906 cholesterol absorption Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- LPTRNLNOHUVQMS-UHFFFAOYSA-N epicatechin Natural products Cc1cc(O)cc2OC(C(O)Cc12)c1ccc(O)c(O)c1 LPTRNLNOHUVQMS-UHFFFAOYSA-N 0.000 description 1
- 235000012734 epicatechin Nutrition 0.000 description 1
- DZYNKLUGCOSVKS-UHFFFAOYSA-N epigallocatechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3cc(O)c(O)c(O)c3 DZYNKLUGCOSVKS-UHFFFAOYSA-N 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 210000002429 large intestine Anatomy 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000019462 natural additive Nutrition 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/82—Theaceae (Tea family), e.g. camellia
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Botany (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Animal Behavior & Ethology (AREA)
- Medicinal Chemistry (AREA)
- Biotechnology (AREA)
- Alternative & Traditional Medicine (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Medical Informatics (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Medicines Containing Plant Substances (AREA)
- Tea And Coffee (AREA)
Abstract
The invention discloses a tea polyphenol extraction method, which comprises the following steps: s1, adding fresh tea leaves and a salt solution into a crusher to crush, and crushing by an ultrasonic cell crusher to obtain tea pulp; s2, uniformly mixing the tea leaf pulp with water to obtain pulp, heating to 60-90 ℃, preserving heat, filtering, and centrifuging by using a high-speed centrifuge to obtain a coarse extract; s3, extracting the crude extract by using an organic solvent, and removing impurities to obtain a tea polyphenol water layer; s4, adsorbing the tea polyphenol water layer by using macroporous adsorption resin, and eluting the resin by using ethyl acetate solution to obtain tea polyphenol eluent; s5, concentrating and drying the tea polyphenol eluent to obtain the tea polyphenol product. The invention overcomes the defects of the prior art, effectively improves the extraction yield of tea polyphenol, and simultaneously avoids the problems of easy oxidation and high impurity content in the extraction process of tea polyphenol.
Description
Technical Field
The invention relates to the technical field of tea polyphenol extraction, and particularly belongs to a tea polyphenol extraction method.
Background
Tea polyphenol is the general name of more than 30 polyphenols in tea, is a polyhydroxy compound which is rich in tea and mainly comprises epicatechin, epigallocatechin, gallate and the like, and the content of the polyhydroxy compound accounts for about 20-30% of the total weight of tea dry matters. The tea polyphenol has multiple active hydroxyl groups (-OH) in its molecule, and can terminate free radical chain reaction in human body, and remove superoxide ion, similar to SOD. The clearance rate of the tea polyphenol to superoxide anions and hydrogen peroxide free radicals reaches more than 98 percent, and the tea polyphenol has obvious dose-effect relationship, and the effect of the tea polyphenol is superior to that of vitamin E and vitamin C. Tea polyphenols also has antibacterial and bactericidal effects, can effectively reduce cholesterol absorption in large intestine, and prevent and treat atherosclerosis, is a strong inhibitor of HIV reverse transcriptase, has immunity enhancing effect, and has anti-tumor, anti-radiation, antioxidant and anti-aging mechanisms. The tea polyphenols are safe and nontoxic, and are natural additives of food, beverage, medicine and cosmetic. At present, tea polyphenol is widely applied to the industries of medicine, beverage, food, health care and the like.
Because tea polyphenol is easy to dissolve in hot water, the existing tea polyphenol extraction process mainly uses hot water as a solution during extraction, but the existing process has poor extraction efficiency, and meanwhile, tea polyphenol is easy to be partially oxidized in the extraction process, so that the quality of a final product is reduced, and the product also contains a large amount of caffeine and other impurities, so that the quality of the tea polyphenol product is seriously influenced.
Disclosure of Invention
The invention aims to provide a tea polyphenol extraction method, which overcomes the problems of low extraction efficiency, oxidized tea polyphenol, low yield and high impurity content in tea polyphenol products in the extraction process of the prior art.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a method for extracting tea polyphenol comprises the following steps:
s1, adding fresh tea leaves and a salt solution into a crusher to crush, and crushing by an ultrasonic cell crusher to obtain tea pulp;
s2, uniformly mixing the tea leaf pulp with water to obtain pulp, heating to 60-90 ℃, preserving heat, filtering, and centrifuging by using a high-speed centrifuge to obtain a coarse extract;
s3, extracting the crude extract by using an organic solvent, and removing impurities to obtain a tea polyphenol water layer;
s4, adsorbing the tea polyphenol water layer by using macroporous adsorption resin, and eluting the resin by using ethyl acetate solution to obtain tea polyphenol eluent;
s5, concentrating and drying the tea polyphenol eluent to obtain the tea polyphenol product.
Preferably, the salt solution is an aqueous solution containing sodium chloride and potassium chloride.
Preferably, the mass fraction of sodium chloride and potassium chloride in the salt solution is 8-11% and 3-7%.
Preferably, the heat preservation process in step S2 further includes a step of using a low-temperature plasma treatment, where the step of using the low-temperature plasma treatment is: and (3) placing the slurry between two electrode plates with the voltage of 12-15KV, and introducing reducing gas into the slurry.
Preferably, the reducing gas is nitrogen containing 5-15% by volume of hydrogen.
Preferably, the organic solvent in step S3 is chloroform containing 0.5-3% by mass of carbon disulfide.
Compared with the prior art, the invention has the following implementation effects:
1. according to the invention, by using the salt solution containing sodium chloride and potassium chloride, the cell walls in the pulp obtained by crushing fresh tea leaves are destroyed through the penetration of ions, and meanwhile, the cell sap in the tea leaves can flow out, and then the tea leaves in the tea pulp can be fully crushed under the action of an ultrasonic cell crusher, so that the dissolution rate of tea polyphenol in the tea leaves is improved, and a large amount of tea polyphenol in the tea pulp is prevented from remaining in residues;
2. by using a low-temperature plasma treatment technology and using inert gas containing hydrogen, under the action of high pressure, hydrogen discharges to generate plasma gas, so that reductive hydrogen ions can be combined with oxidizing substances in the crude extract, the tea polyphenol in the crude extract is prevented from being oxidized in the heating process, and the tea polyphenol partially oxidized under the action of crushing and an ultrasonic cell crusher is reduced again, so that the problem of reduced quality of the tea polyphenol product caused by oxidation in the process of extracting the tea polyphenol is effectively solved.
3. Under the condition that common chloroform is used as an extracting agent, carbon disulfide is added into the chloroform to serve as a synergist, and the carbon disulfide has a synergistic effect, so that the extraction efficiency during chloroform extraction is improved, the extraction time is shortened, the content of impurities such as caffeine in tea polyphenol is reduced, and the purity of the tea polyphenol is improved.
4. The extraction method effectively improves the extraction yield of the tea polyphenol, and simultaneously avoids the problems of easy oxidation and high impurity content in the extraction process of the tea polyphenol.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adding 20kg of fresh tea leaf Jinzhaicui eyebrow and 10kg of salt solution containing sodium chloride and potassium chloride with the mass fractions of 10% and 4% into a crusher for crushing, and crushing for 30min by using a 3KW ultrasonic cell crusher to obtain tea leaf pulp; then, tea slurry was uniformly mixed with 40kg of water to obtain slurry, the slurry was placed in a glass container between two electrode plates at a voltage of 15KV, and nitrogen gas containing 13% by volume of hydrogen gas was introduced into the slurry at a gas flow rate of 3m3Heating to 70 deg.C for 40min, filtering, and centrifuging at 20000 rpm to obtain crude extract.
Then, extracting the crude extract for 25min by using a chloroform solution containing 1.2% of carbon disulfide by mass percent, wherein the volume ratio of the crude extract to the chloroform solution is 1:1.5, and removing impurities to obtain a tea polyphenol water layer;
finally, adsorbing the tea polyphenol water layer by using macroporous adsorption resin, and eluting the resin by using ethyl acetate solution to obtain tea polyphenol eluent; then, the tea polyphenol eluent is concentrated and dried to obtain 5.77kg of tea polyphenol products.
Example 2
20kg of fresh tea leaves, JinzhaicuimeiAdding 10kg of salt solution containing 9% and 3% of sodium chloride and potassium chloride into a pulverizer for pulverizing, and then pulverizing for 30min by using a 3KW ultrasonic cell crusher to obtain tea pulp; then, tea slurry was uniformly mixed with 40kg of water to obtain slurry, the slurry was placed in a glass container between two electrode plates at a voltage of 12KV, and nitrogen gas containing 15% by volume of hydrogen gas was introduced into the slurry at a gas flow rate of 4m3Heating to 80 deg.C for 60min, filtering, and centrifuging at 20000 rpm to obtain crude extract.
Then, extracting the crude extract for 20min by using a chloroform solution containing 3% of carbon disulfide by mass percent, wherein the volume ratio of the crude extract to the chloroform solution is 1:1.5, and removing impurities to obtain a tea polyphenol water layer;
finally, adsorbing the tea polyphenol water layer by using macroporous adsorption resin, and eluting the resin by using ethyl acetate solution to obtain tea polyphenol eluent; then, the tea polyphenol eluent is concentrated and dried to obtain 5.83kg of tea polyphenol products.
Comparative example 1
The difference from example 1 is that the salt solution added during the pulverization process does not contain sodium chloride and potassium chloride, and 4.62kg of tea polyphenol is finally obtained.
Comparative example 2
The difference from example 1 is that the voltage between the electrode plates is 0, and 4.80kg of tea polyphenol is finally obtained.
Comparative example 3
The difference from example 1 is that the chloroform solution does not contain carbon disulfide, and 5.92kg of tea polyphenol is finally obtained.
The tea polyphenol products of examples 1-2 and comparative examples 1-3 were tested for purity and caffeine content according to the method of GB/T8313-:
example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
Purity of tea polyphenols% | 96.4 | 97.2 | 94.3 | 87.8 | 91.7 |
Content of caffeine% | 0.18 | 0.15 | 0.23 | 0.36 | 1.82 |
According to the yield contrast, the purity and the content of caffeine of the tea polyphenol, the salt solution is used as the solvent for auxiliary crushing, so that the residual quantity of the tea polyphenol in tea leaf residues is effectively reduced, the yield of the tea polyphenol is improved, meanwhile, the problem that the tea polyphenol is easily oxidized in the dissolving process is effectively solved by using low-temperature plasma treatment, the content of impurities is reduced, and meanwhile, the carbon disulfide is used as a synergist, so that the purity of the tea polyphenol is effectively improved, and the content of caffeine is reduced.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A tea polyphenol extraction method is characterized by comprising the following steps:
s1, adding fresh tea leaves and a salt solution into a crusher to crush, and crushing by an ultrasonic cell crusher to obtain tea pulp;
s2, uniformly mixing the tea leaf pulp with water to obtain pulp, heating to 60-90 ℃, preserving heat, filtering, and centrifuging by using a high-speed centrifuge to obtain a coarse extract;
s3, extracting the crude extract by using an organic solvent, and removing impurities to obtain a tea polyphenol water layer;
s4, adsorbing the tea polyphenol water layer by using macroporous adsorption resin, and eluting the resin by using ethyl acetate solution to obtain tea polyphenol eluent;
s5, concentrating and drying the tea polyphenol eluent to obtain the tea polyphenol product.
2. The method for extracting tea polyphenol as claimed in claim 1, wherein: the salt solution is an aqueous solution containing sodium chloride and potassium chloride.
3. The method for extracting tea polyphenol as claimed in claim 2, wherein: the mass fractions of sodium chloride and potassium chloride in the salt solution are 8-11% and 3-7%.
4. The method for extracting tea polyphenol as claimed in claim 1, wherein: the step S2 of performing a heat preservation process further includes a step of performing a low-temperature plasma treatment, where the step of performing the low-temperature plasma treatment includes: and (3) placing the slurry between two electrode plates with the voltage of 12-15KV, and introducing reducing gas into the slurry.
5. The method for extracting tea polyphenol as claimed in claim 4, wherein: the reducing gas is nitrogen containing 5-15% hydrogen by volume.
6. The method for extracting tea polyphenol as claimed in claim 1, wherein: the organic solvent in step S4 is chloroform containing 0.5-3% by mass of carbon disulfide.
Priority Applications (1)
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CN202011353114.6A CN112245506A (en) | 2020-11-26 | 2020-11-26 | Tea polyphenol extraction method |
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CN202011353114.6A CN112245506A (en) | 2020-11-26 | 2020-11-26 | Tea polyphenol extraction method |
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CN112245506A true CN112245506A (en) | 2021-01-22 |
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CN202011353114.6A Withdrawn CN112245506A (en) | 2020-11-26 | 2020-11-26 | Tea polyphenol extraction method |
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2020
- 2020-11-26 CN CN202011353114.6A patent/CN112245506A/en not_active Withdrawn
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Application publication date: 20210122 |