CN112245506A - Tea polyphenol extraction method - Google Patents

Tea polyphenol extraction method Download PDF

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Publication number
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
pulp
extracting
polyphenol
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CN202011353114.6A
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杨玉兰
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Jinzhai Yuye Agricultural Products Sales Co ltd
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Jinzhai Yuye Agricultural Products Sales Co ltd
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Priority to CN202011353114.6A priority Critical patent/CN112245506A/en
Publication of CN112245506A publication Critical patent/CN112245506A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/82Theaceae (Tea family), e.g. camellia
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

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  • 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

Tea polyphenol extraction method
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.
CN202011353114.6A 2020-11-26 2020-11-26 Tea polyphenol extraction method Withdrawn CN112245506A (en)

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Application Number Priority Date Filing Date Title
CN202011353114.6A CN112245506A (en) 2020-11-26 2020-11-26 Tea polyphenol extraction method

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Application Number Priority Date Filing Date Title
CN202011353114.6A CN112245506A (en) 2020-11-26 2020-11-26 Tea polyphenol extraction method

Publications (1)

Publication Number Publication Date
CN112245506A true CN112245506A (en) 2021-01-22

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Application publication date: 20210122