CN112823780A - Extraction method of tea polyphenol - Google Patents

Extraction method of tea polyphenol Download PDF

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Publication number
CN112823780A
CN112823780A CN201911150741.7A CN201911150741A CN112823780A CN 112823780 A CN112823780 A CN 112823780A CN 201911150741 A CN201911150741 A CN 201911150741A CN 112823780 A CN112823780 A CN 112823780A
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tea polyphenol
extraction
extracting solution
filter cake
raw material
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龙永久
王代军
王栓来
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Hunan Qinong Biotechnology Co Ltd
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Hunan Qinong Biotechnology Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • 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
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/02Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/10Washing or bathing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair
    • 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/19Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
    • 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
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
    • A61K2800/522Antioxidants; Radical scavengers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52Stabilizers
    • A61K2800/524Preservatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/82Preparation or application process involves sonication or ultrasonication

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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Abstract

A method for extracting tea polyphenol sequentially comprises the following steps: (1) adding water and cellulase into a raw material containing tea polyphenol, carrying out enzymolysis, and filtering to obtain a filter cake and a first extracting solution; (2) adding ethanol into the filter cake for extraction, and filtering to obtain a second extracting solution; (3) and combining the first extracting solution and the second extracting solution, and then separating to obtain the tea polyphenol. The method has short extraction time, high extraction rate, and no oxidation of tea polyphenols.

Description

Extraction method of tea polyphenol
Technical Field
The invention belongs to the technical field of tea polyphenol extraction.
Background
Tea polyphenols are the general name of polyphenols in tea, and are white amorphous powder, which are easily soluble in water, soluble in ethanol, methanol, acetone, ethyl acetate, and insoluble in chloroform. The green tea has high tea polyphenol content accounting for 15-30% of the weight, and the tea polyphenol comprises the following main components: flavanones, anthocyanidins, flavonols, anthocyanins, phenolic acids and depside 6 compounds.
The tea polyphenol as an excellent additive of cosmetics and daily necessities has the following remarkable effects: has strong antibacterial and oxidase inhibiting effects, and can be used for preventing and treating dermatoses, skin allergy, skin pigmentation, wrinkle, dental caries, dental plaque, periodontitis, and halitosis. The tea polyphenol can be used as antioxidant, quality guaranteeing agent, anti-wrinkle agent, skin whitening agent, radiation protection agent, sunscreen agent, special cosmetic additive and the like on cosmetics and daily necessities, and can be used on daily cosmetics such as bath soap, bath lotion, shampoo, detergent, toothpaste, tooth powder, mouthwash, anti-halitosis agent and the like to increase the functions of the products.
At present, the main extraction methods of tea polyphenol comprise the following steps: the first is organic solvent extraction: this is one of the most widely used methods. The principle is that the solubility difference of different compounds in different solvents in tea is utilized for extraction and separation, the method is simple, the extraction rate of tea polyphenol is 10-15%, and the process flow is as follows: tea → extraction with boiling water → filtration → filtrate → extraction with chloroform → extraction with ethyl acetate → concentrated drying → crude GTP; the process has the following disadvantages: a plurality of organic solvents are used in the whole production process, and the using amount of the organic solvents is large; the process is complicated, multiple times of distillation are needed, the heating time is too long, and the tea polyphenol is easy to oxidize. The other is ion precipitation extraction method, which mainly utilizes some metal ions to precipitate tea polyphenol so as to separate the tea polyphenol from caffeine. The method is characterized in that: after the tea is leached by hot water, a precipitator is added to obtain crystalline precipitates of tea polyphenol and metal ions, the leaching liquor does not need to be concentrated, the energy consumption can be reduced to a certain extent, meanwhile, because the selectivity of the precipitates is high, the purity of the product can relatively better reach more than 85 percent, but the loss of the tea polyphenol is large in the subsequent dilute acid conversion and dissolution process, and some precipitants are metal ions with certain toxicity, and some precipitants are alkaline and easily cause the oxidation of the tea polyphenol. There are also adsorption separation extraction method, supercritical fluid extraction, etc., but the techniques are not well developed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for extracting tea polyphenol, which sequentially comprises the following steps:
(1) adding water and cellulase into a raw material containing tea polyphenol, carrying out enzymolysis, and filtering to obtain a filter cake and a first extracting solution;
(2) adding ethanol into the filter cake for extraction, and filtering to obtain a second extracting solution;
(3) and combining the first extracting solution and the second extracting solution, and then separating to obtain the tea polyphenol.
Wherein, the weight ratio of the cellulase to the raw material containing tea polyphenol in the step (1) is (0.5-0.9): 100; the enzymolysis temperature is normal temperature; the weight ratio of water to the raw material containing tea polyphenol is (5-8): 1. The cellulase is added in the extraction process to destroy the structure of the cell wall, so that the cell wall is locally collapsed, dissolved and loosened, thereby reducing the resistance from the cell wall and intercellular substance during solvent extraction, accelerating the speed of the effective components for dissolving out the cells, improving the extraction efficiency and shortening the extraction time.
Wherein the weight ratio of the ethanol to the filter cake in the step (2) is 3-5: 1.
Concentrating the first extract and the second extract in the step (3), and separating by using macroporous adsorption resin to obtain a pure tea polyphenol product;
more preferably, in the enzymolysis process in the step (1), ultrasonic waves are adopted for auxiliary extraction, the power is 150-.
More preferably, the first extract and the second extract are decolorized with activated carbon before being concentrated.
The invention has the following beneficial effects:
(1) the cellulase is added in the extraction process to destroy the structure of the cell wall, so that the cell wall is locally collapsed, dissolved and loosened, thereby reducing the resistance from the cell wall, the intercellular substance and the like during solvent extraction, accelerating the speed of dissolving out the effective components from the cells, shortening the extraction time and improving the extraction efficiency.
(2) Ultrasonic wave is adopted for auxiliary extraction, and the diffusion of tea polyphenol to a solvent is accelerated by utilizing the mechanical crushing and cavitation of the ultrasonic wave, so that the extraction rate of effective components is increased, and the extraction time is shortened.
(3) The cellulase and the ultrasonic wave are adopted for synchronous extraction, and normal-temperature extraction can be carried out, so that the oxidation of tea polyphenol is avoided, and the product quality is improved.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to be limiting.
Example 1
(1) Adding water and cellulase into a raw material containing tea polyphenol, carrying out enzymolysis, and filtering to obtain a filter cake and a first extracting solution;
(2) adding ethanol into the filter cake for extraction, and filtering to obtain a second extracting solution;
(3) and combining the first extracting solution and the second extracting solution, and then separating to obtain the tea polyphenol.
Wherein the weight ratio of the cellulase to the raw material containing tea polyphenol in the step (1) is 0.5: 100; the enzymolysis temperature is normal temperature; the weight ratio of the water to the raw material containing tea polyphenol is 7: 1; wherein the weight ratio of the ethanol to the filter cake in the step (2) is 4: 1; in the enzymolysis process in the step (1), ultrasonic waves are adopted for auxiliary extraction, the power is 200W, and the service time of the ultrasonic waves is 25 min.
Concentrating the first extract and the second extract in the step (3), and separating by using macroporous adsorption resin to obtain a pure tea polyphenol product; and performing activated carbon decolorization treatment before concentrating the first extracting solution and the second extracting solution.
Example 2
(1) Adding water and cellulase into a raw material containing tea polyphenol, carrying out enzymolysis, and filtering to obtain a filter cake and a first extracting solution;
(2) adding ethanol into the filter cake for extraction, and filtering to obtain a second extracting solution;
(3) and combining the first extracting solution and the second extracting solution, and then separating to obtain the tea polyphenol.
Wherein the weight ratio of the cellulase to the raw material containing tea polyphenol in the step (1) is 0.8: 100; the enzymolysis temperature is normal temperature; the weight ratio of the water to the raw material containing tea polyphenol is 7: 1; wherein the weight ratio of the ethanol to the filter cake in the step (2) is 3: 1; in the enzymolysis process in the step (1), ultrasonic waves are adopted for auxiliary extraction, the power is 150W, and the service time of the ultrasonic waves is 29 min.
Concentrating the first extract and the second extract in the step (3), and separating by using macroporous adsorption resin to obtain a pure tea polyphenol product; and performing activated carbon decolorization treatment before concentrating the first extracting solution and the second extracting solution.
Example 3
(1) Adding water and cellulase into a raw material containing tea polyphenol, carrying out enzymolysis, and filtering to obtain a filter cake and a first extracting solution;
(2) adding ethanol into the filter cake for extraction, and filtering to obtain a second extracting solution;
(3) and combining the first extracting solution and the second extracting solution, and then separating to obtain the tea polyphenol.
Wherein the weight ratio of the cellulase to the raw material containing tea polyphenol in the step (1) is 0.7: 100; the enzymolysis temperature is normal temperature; the weight ratio of the water to the raw material containing tea polyphenol is 6: 1; wherein the weight ratio of the ethanol to the filter cake in the step (2) is 5: 1; in the enzymolysis process in the step (1), ultrasonic waves are adopted for auxiliary extraction, the power is 150W, and the service time of the ultrasonic waves is 27 min.
Concentrating the first extract and the second extract in the step (3), and separating by using macroporous adsorption resin to obtain a pure tea polyphenol product; and performing activated carbon decolorization treatment before concentrating the first extracting solution and the second extracting solution.
The purity of the tea polyphenol extract obtained in the above examples 1-3 was about 98%, and the extraction rates of the extract were 29.8%, 30.2% and 28.7%, respectively.

Claims (5)

1. The extraction method of tea polyphenol is characterized by sequentially comprising the following steps:
(1) adding water and cellulase into a raw material containing tea polyphenol, carrying out enzymolysis, and filtering to obtain a filter cake and a first extracting solution;
(2) adding ethanol into the filter cake for extraction, and filtering to obtain a second extracting solution;
(3) mixing the first and second extractive solutions, and separating to obtain tea polyphenols;
wherein in the enzymolysis process in the step (1), ultrasonic waves are adopted for auxiliary extraction.
2. The method for extracting tea polyphenol as claimed in claim 1, wherein the weight ratio of the cellulase to the raw material containing tea polyphenol in step (1) is (0.5-0.9): 100; the enzymolysis temperature is normal temperature; the weight ratio of water to the raw material containing tea polyphenol is (5-8): 1.
3. The method for extracting tea polyphenol as claimed in claim 1, wherein the weight ratio of the ethanol to the filter cake in the step (2) is 3-5: 1.
4. The method as claimed in claim 1, wherein the ultrasonic power is 150-200W.
5. The method for extracting tea polyphenols according to claim 1, wherein the ultrasonic wave is used for 20-30 min.
CN201911150741.7A 2019-11-21 2019-11-21 Extraction method of tea polyphenol Pending CN112823780A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106943768A (en) * 2017-04-01 2017-07-14 北京国康本草物种生物科学技术研究院有限公司 Tea Polyphenols and its extracting method and application
CN108576311A (en) * 2018-03-08 2018-09-28 陕西师范大学 A kind of method of negative pressure-ultrasonic wave added cellulase hydrolysis extraction Fu-brick tea polyphenol

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106943768A (en) * 2017-04-01 2017-07-14 北京国康本草物种生物科学技术研究院有限公司 Tea Polyphenols and its extracting method and application
CN108576311A (en) * 2018-03-08 2018-09-28 陕西师范大学 A kind of method of negative pressure-ultrasonic wave added cellulase hydrolysis extraction Fu-brick tea polyphenol

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Application publication date: 20210521