CN113041188A - Method for extracting tea polyphenol for cosmetics - Google Patents
Method for extracting tea polyphenol for cosmetics Download PDFInfo
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- CN113041188A CN113041188A CN202110293392.5A CN202110293392A CN113041188A CN 113041188 A CN113041188 A CN 113041188A CN 202110293392 A CN202110293392 A CN 202110293392A CN 113041188 A CN113041188 A CN 113041188A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics 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
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
- A61K8/498—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/74—Biological properties of particular ingredients
- A61K2800/78—Enzyme modulators, e.g. Enzyme agonists
- A61K2800/782—Enzyme inhibitors; Enzyme antagonists
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Dermatology (AREA)
- Engineering & Computer Science (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a method for extracting tea polyphenol for cosmetics, and belongs to the technical field of plant extraction processes. It comprises the following steps: (1) pre-treating; (2) polyvinyl alcohol treatment: transferring the mixture into a reaction tank, adding a polyvinyl alcohol solution for soaking, and washing with clear water after soaking; (3) drying treatment: transferring the mixture into a low-temperature drying box for drying; (4) and (3) crushing treatment: transferring to a crusher for crushing; (5) and (3) coarse extraction treatment: transferring to a reaction kettle, adding enzyme liquid, performing enzymolysis reaction, and centrifuging to recover clear liquid; (6) fine extraction treatment: transferring to supercritical carbon dioxide extraction device, and recovering tea polyphenol slurry; (7) secondary extraction treatment: selecting macroporous adsorption resin to adsorb impurities, and recovering effluent liquid; (8) and (5) performing freeze drying treatment. Tests show that the parameters of tea polyphenol extraction purity, extraction rate, DPPH free radical clearance rate and the like have better significant differences.
Description
Technical Field
The invention belongs to the technical field of plant extraction processes, and particularly relates to a method for extracting tea polyphenol for cosmetics.
Background
The tea polyphenol is extracted from tea leaves, has a relatively comprehensive effect, and the content of the tea polyphenol in the tea leaves is 20-30%. Tea polyphenols have strong antioxidant effect, and can inhibit collagenase and elastase, prevent elastin content from decreasing or denaturing, maintain skin elasticity, and prevent wrinkle. The tea polyphenols can absorb ultraviolet ray, reduce melanin growth, and inhibit tyrosinase and peroxidase, thereby whitening skin. Polyphenols are natural products having strong absorption in the ultraviolet region and are non-toxic to humans. Through the compounding of several kinds of polyphenol and flavone, the natural ultraviolet absorbent with broad spectrum and sun protection can be obtained by utilizing the difference of the absorption of ultraviolet regions, and the effects of reducing the formation of skin melanin and preventing skin aging are achieved.
The prior art, such as Chinese invention patent, application number: CN201810334647.6, publication No.: CN108272695B discloses a method for extracting tea polyphenol for cosmetics, which comprises the steps of raw material treatment, ultrasonic treatment, supercritical CO2 extraction, purification and the like. However, the above patent has many problems by analysis: the problems of water bath heating during raw material treatment, cooling and heat dissipation of a solution during ultrasonic treatment, too complex supercritical carbon dioxide extraction process, lack of effective pretreatment steps for raw materials and the like are not considered.
Disclosure of Invention
1. Problems to be solved
Aiming at the problems in the prior art, the invention provides the method for extracting the tea polyphenol for the cosmetics, and the parameters such as the extraction purity, the extraction rate, the removal rate of DPPH free radicals and the like of the tea polyphenol have better significant difference. The antioxidant can be added into cosmetics as an antioxidant after preliminary testing.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A method for extracting tea polyphenols for cosmetic comprises the following steps:
(1) pretreatment: preparing tea leaves, removing impurities on the surfaces of the tea leaves, cleaning and airing;
(2) polyvinyl alcohol treatment: transferring the tea leaves pretreated in the step (1) into a reaction tank, adding a polyvinyl alcohol solution for soaking, and washing with clear water after soaking;
(3) drying treatment: transferring the tea leaves treated by the polyvinyl alcohol in the step (2) into a low-temperature drying oven for drying;
(4) and (3) crushing treatment: selecting the tea leaves dried in the step (3), and transferring the tea leaves to a crusher for crushing;
(5) and (3) coarse extraction treatment: selecting the tea leaves crushed in the step (4), transferring the tea leaves into a reaction kettle, adding enzyme liquid, performing enzymolysis reaction, and centrifuging to recover clear liquid;
(6) fine extraction treatment: selecting the clear liquid obtained after the crude extraction in the step (5), transferring the clear liquid into a supercritical carbon dioxide extraction device, and recovering tea polyphenol slurry;
(7) secondary extraction treatment: selecting the tea polyphenol slurry after fine extraction in the step (6), selecting macroporous adsorption resin for impurity adsorption, and recovering effluent liquid;
(8) and (3) freeze drying treatment: and (4) selecting the effluent liquid obtained after the secondary extraction treatment in the step (7), conveying the effluent liquid into a vacuum freeze dryer, and pulverizing to obtain the powder.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the variety of the tea in the step (1) is Meng Hai big leaf tea;
the impurities on the surface of the tea in the step (1) comprise soil particles, stone particles, dust and silt, and the impurities are removed by adopting a winnowing machine for screening; wherein the average wind speed of the air supply outlet of the air separator is 0.90m3(s), wherein the internal air pressure of the air separator is 300Pa, and the air separator; wherein before the tea leaves are loaded into the winnowing machine, a plurality of tea leaves are connected with the same tea stem for manual separation;
the cleaning mode in the step (1) is to soak the tea leaves by adopting warm water, the soaking time is controlled to be 20min, the temperature of the warm water is controlled to be 15 ℃, meanwhile, a stirrer is adopted to stir the soaked tea leaves, and the rotating speed of blades of the stirrer is controlled to be 20 r/min;
the drying mode in the step (1) is that the cleaned tea leaves are placed on a bamboo sieve and are naturally dried in the shade or dried by a fan, the time for naturally drying the tea leaves or the dried tea leaves by the fan is controlled within 4 hours, and the temperature of the shade is controlled within 20 ℃ during naturally drying or drying by the fan.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the mass concentration of the polyvinyl alcohol solution in the step (2) is 10 percent;
controlling the temperature of the polyvinyl alcohol solution in the step (2) to be 25 ℃;
the soaking time of the polyvinyl alcohol solution in the step (2) is controlled to be 60 min;
and (3) the clean water in the step (2) is deionized water.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the low-temperature drying box in the step (3) is a blast type drying box;
the drying temperature in the step (3) is 40 ℃;
the drying time in the step (3) is 1 h.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the pulverizer in the step (4) is an airflow pulverizer;
controlling the working medium pressure of the pulverizer in the step (4) to be 0.4 MPa;
the average particle size of the crushed tea leaves in the step (4) is controlled to be 300 meshes.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
in the step (5), the enzyme solution is an aqueous solution containing cellulase, amylase, catalase and elastase, wherein the mass concentration of the enzyme solution is 3mg/mL, and the dosage ratio of the cellulase, the amylase, the catalase and the elastase is 1: 5: 3: 6;
the temperature of the enzymolysis reaction in the step (5) is 37 ℃.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the centrifugal equipment in the step (5) is an ultracentrifuge;
the centrifugal force of the centrifugation in the step (5) is 100000 Xg;
the centrifugation time in the step (5) is 30 min;
the temperature of the centrifugation in the step (5) was 4 ℃.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the model of the supercritical carbon dioxide extraction equipment in the step (6) is HA121-50-01, and the manufacturer is Jiangsu Nantong Huaan supercritical extraction company Limited;
the pressure of the supercritical carbon dioxide extraction in the step (6) is 21 MPa;
the temperature of the supercritical carbon dioxide extraction in the step (6) is 43 ℃;
the time of supercritical carbon dioxide extraction in step (6) is 20 min.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
adding an auxiliary agent into the carbon dioxide fluid of the supercritical carbon dioxide in the step (6), wherein the auxiliary agent is a mixture of ethyl acetate, propane and isopropyl ether, and the mass ratio of the ethyl acetate to the propane to the isopropyl ether is 3: 2: 2.
in the above-mentioned extraction method of tea polyphenol for cosmetics,
the sample loading flow rate of the macroporous adsorption resin in the step (7) is 1 BV/h;
the model of the macroporous adsorption resin in the step (7) is LX-8, which is purchased from Xian lan Xiao science and technology New materials GmbH.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
the extraction method of the invention has better significant differences in the parameters of tea polyphenol extraction purity, extraction rate, DPPH free radical clearance rate and the like. In the prior art, the invention sets key parameters of enzymolysis, and when the dosage ratio of cellulase, amylase, catalase and elastase is 1: 5: 3: 6, the extraction purity of the tea polyphenol can be effectively optimized, and meanwhile, an organic auxiliary agent is innovatively introduced, wherein the auxiliary agent is a mixture of ethyl acetate, propane and isopropyl ether, and the mass ratio of ethyl acetate to propane to isopropyl ether is 3: 2: 2, the extraction purity of the tea polyphenol is greatly improved; in addition, compared with a plurality of prior arts, the average value of the extraction purity of the tea polyphenol is 92.6%, the extraction rate of the tea polyphenol is 32.1%, and the scavenging rate of DPPH free radicals is up to 89.4%.
Drawings
FIG. 1 is a process flow diagram of the extraction method of tea polyphenol for cosmetics according to the present invention.
Detailed Description
The invention is further described with reference to specific examples.
Example 1
As shown in fig. 1, the method for extracting tea polyphenol for cosmetics according to this embodiment includes the following steps:
(1) pretreatment: preparing tea leaves, removing impurities on the surfaces of the tea leaves, cleaning and airing;
(2) polyvinyl alcohol treatment: transferring the tea leaves pretreated in the step (1) into a reaction tank, adding a polyvinyl alcohol solution for soaking, and washing with clear water after soaking;
(3) drying treatment: transferring the tea leaves treated by the polyvinyl alcohol in the step (2) into a low-temperature drying oven for drying;
(4) and (3) crushing treatment: selecting the tea leaves dried in the step (3), and transferring the tea leaves to a crusher for crushing;
(5) and (3) coarse extraction treatment: selecting the tea leaves crushed in the step (4), transferring the tea leaves into a reaction kettle, adding enzyme liquid, performing enzymolysis reaction, and centrifuging to recover clear liquid;
(6) fine extraction treatment: selecting the clear liquid obtained after the crude extraction in the step (5), transferring the clear liquid into a supercritical carbon dioxide extraction device, and recovering tea polyphenol slurry;
(7) secondary extraction treatment: selecting the tea polyphenol slurry after fine extraction in the step (6), selecting macroporous adsorption resin for impurity adsorption, and recovering effluent liquid;
(8) and (3) freeze drying treatment: and (4) selecting the effluent liquid obtained after the secondary extraction treatment in the step (7), conveying the effluent liquid into a vacuum freeze dryer, and pulverizing to obtain the powder.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the variety of the tea in the step (1) is Meng Hai big leaf tea;
the impurities on the surface of the tea in the step (1) comprise soil particles, stone particles, dust and silt, and the impurities are removed by adopting a winnowing machine for screening; wherein the average wind speed of the air supply outlet of the air separator is 0.90m3/sWherein the internal wind pressure of the air separator is 300Pa, and the air separator is arranged; wherein before the tea leaves are loaded into the winnowing machine, a plurality of tea leaves are connected with the same tea stem for manual separation;
the cleaning mode in the step (1) is to soak the tea leaves by adopting warm water, the soaking time is controlled to be 20min, the temperature of the warm water is controlled to be 15 ℃, meanwhile, a stirrer is adopted to stir the soaked tea leaves, and the rotating speed of blades of the stirrer is controlled to be 20 r/min;
the drying mode in the step (1) is that the cleaned tea leaves are placed on a bamboo sieve and are naturally dried in the shade or dried by a fan, the time for naturally drying the tea leaves or the dried tea leaves by the fan is controlled within 4 hours, and the temperature of the shade is controlled within 20 ℃ during naturally drying or drying by the fan.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the mass concentration of the polyvinyl alcohol solution in the step (2) is 10 percent;
controlling the temperature of the polyvinyl alcohol solution in the step (2) to be 25 ℃;
the soaking time of the polyvinyl alcohol solution in the step (2) is controlled to be 60 min;
and (3) the clean water in the step (2) is deionized water.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the low-temperature drying box in the step (3) is a blast type drying box;
the drying temperature in the step (3) is 40 ℃;
the drying time in the step (3) is 1 h.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the pulverizer in the step (4) is an airflow pulverizer;
controlling the working medium pressure of the pulverizer in the step (4) to be 0.4 MPa;
the average particle size of the crushed tea leaves in the step (4) is controlled to be 300 meshes.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
in the step (5), the enzyme solution is an aqueous solution containing cellulase, amylase, peroxidase and elastase, wherein the mass concentration of the enzyme solution is 3mg/mL, and the dosage ratio of the cellulase, the amylase, the catalase and the elastase is 1: 5: 3: 6; wherein, the cellulase, amylase, catalase and elastase are purchased from Shandong Longglong bioengineering Co., Ltd;
the temperature of the enzymolysis reaction in the step (5) is 37 ℃.
The selection of the four enzymes in the enzyme solution is optimized for multiple times, and the enzyme solution is cooperated with the research and development department and the quality inspection department of a factory and the biological key laboratory of Zhejiang university in multiple directions in the treatment process. Referring to a large number of documents, it has been found that the selection of the four enzymes mentioned above is optimized in this application by a large number of tests, typically prior to the extraction of tea polyphenols in the process, especially by supercritical or subcritical extraction. As shown in Table 1, the content of tea polyphenols was measured by the following method (Yuan-supercritical CO)2Study on copper, lead and cadmium in green tea by complex extraction and influence on tea polyphenols and caffeine [ D]Wuhan university), it can be obviously found that the components have a synergistic effect, and the combination effect is difficult to achieve by removing one component alone.
TABLE 1 influence of the ratio of the amounts of different components in the enzyme solution on the extraction purity of tea polyphenols
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the centrifugal equipment in the step (5) is an ultracentrifuge;
the centrifugal force of the centrifugation in the step (5) is 100000 Xg;
the centrifugation time in the step (5) is 30 min;
the temperature of the centrifugation in the step (5) was 4 ℃.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the model of the supercritical carbon dioxide extraction equipment in the step (6) is HA121-50-01, and the manufacturer is Jiangsu Nantong Huaan supercritical extraction company Limited;
the pressure of the supercritical carbon dioxide extraction in the step (6) is 21 MPa;
the temperature of the supercritical carbon dioxide extraction in the step (6) is 43 ℃;
the time of supercritical carbon dioxide extraction in step (6) is 20 min.
In the above-mentioned extraction method of tea polyphenol for cosmetics,
adding an auxiliary agent into the carbon dioxide fluid of the supercritical carbon dioxide in the step (6), wherein the auxiliary agent is a mixture of ethyl acetate, propane and isopropyl ether, and the mass ratio of the ethyl acetate to the propane to the isopropyl ether is 3: 2: 2. it should be noted that the mass usage of the auxiliary agent is 10% of the mass usage of the carbon dioxide fluid.
It should be noted that the selection of the carbon dioxide fluid is also very critical, and in the process of searching, we find that there are fresh added auxiliary agents, and according to some research reports abroad, the addition of a proper organic reagent into the carbon dioxide fluid has the effect of promoting the extraction of tea polyphenols, but what kind of organic auxiliary agents and kinds and dosage ratios of the organic auxiliary agents are specifically selected is very critical, and not only the interaction between the organic auxiliary agents and the carbon dioxide fluid but also the interaction between the tea polyphenols and the organic auxiliary agents need to be considered, and the chemical structure properties of the tea polyphenols are involved. As shown in Table 2, the three substances of ethyl acetate, propane and isopropyl ether interact with each other to realize synergistic interaction, so that the extraction purity of the tea polyphenol can be improved, and no related similar research is found.
TABLE 2 Effect of organic auxiliary on tea Polyphenol extraction purity
In the above-mentioned extraction method of tea polyphenol for cosmetics,
the sample loading flow rate of the macroporous adsorption resin in the step (7) is 1 BV/h;
the model of the macroporous adsorption resin in the step (7) is LX-8, which is purchased from Xian lan Xiao science and technology New materials GmbH;
the specific use method of the macroporous adsorption resin is as follows:
column packing (adopting wet column packing):
A. laboratory
Measuring: and mixing a certain amount of resin and deionized water in a beaker, then pouring the mixed resin aqueous solution into a measuring cylinder to ensure that the resin is fully settled, and supplementing and transferring to ensure that a resin bed layer is level with corresponding scales, thus finishing the measurement of the resin.
Filling: closing an outlet valve at the lower end of the ion exchange column, introducing all the resin in the measuring cylinder into the ion exchange column by using water, then opening the outlet valve of the ion exchange column to enable the resin to be settled and compacted in the column, and then closing the outlet valve of the ion exchange column for later use. (Note: the liquid level should be kept 1-2cm higher than the resin bed to avoid dry column.)
B. Industrialization
Before the new resin is filled into the column, clean water and alkali liquor are used for cleaning the relevant pipelines of the resin exchange column, and solid waste materials such as welding slag and dust and other impurities attached to the wall and the wall of the column are cleaned. Then 1/3 volumes of water were injected into the column, a small amount of resin was taken and the resin was loaded into the column from the top manhole of the exchange column. Closing a manhole, injecting water into the column, simultaneously opening a drainage valve at the lower part of the exchange column, intercepting at a drainage port by using a screen with the diameter of more than or equal to 80 meshes, and observing whether resin leaks or not, wherein if individual small particles exist, the normal phenomenon is achieved; if large-particle resin appears and the amount is more, the problem of the lower filter plate of the exchange column is solved, the resin and water are discharged, the welding line and the water cap of the lower filter plate are checked, the reason is found, and the lower filter plate is overhauled. After the overhaul is finished, the detection is carried out according to the method until the requirement is met, and then the residual resin is added into the exchange column.
After the resin is filled into the column, reversely cleaning the resin by using deionized water, controlling the cleaning flow rate at 3BV/h, cleaning for about 1h, and stopping water washing to ensure that the resin is naturally and completely settled; and then, positively cleaning the resin column bed by using deionized water, controlling the cleaning flow rate to be 5BV/h, and stopping after about 1h of cleaning.
Resin pretreatment:
firstly, carrying out column treatment by using a 4% sodium hydroxide solution, wherein the treatment flow rate is controlled to be 2BV/h, and the treatment capacity is 3 BV; and after the treatment is finished, using deionized water to pass through the column to clean the residual alkali in the column bed and the resin pore channel until the pH value of the outlet liquid is less than or equal to 10, stopping water washing, and at least reserving a liquid level layer of 20-30cm on the resin bed layer to prevent the column from being dried.
Then, carrying out column passing treatment by using a 4% hydrochloric acid solution, wherein the treatment flow rate is controlled to be 2BV/h, and the treatment capacity is 3 BV; and after the treatment is finished, passing deionized water through the column to clean the column bed and residual acid in the resin pore channel until the pH value of the outlet liquid is more than or equal to 4, stopping water washing, and at least reserving a liquid level layer of 20-30cm on the resin bed layer to prevent the column from being dried.
Soaking the resin in the column with 95% ethanol solution for 3h, and treating with the same ethanol solution at a flow rate of 2BV/h and a treatment capacity of 2BV until the effluent is diluted with one time of water in a test tube and is not turbid. Finally, deionized water is used for passing through the column for cleaning,
stopping cleaning until the ethanol content at the outlet is less than 1% or no obvious ethanol smell exists, and reserving a liquid surface layer of at least 20-30cm on the resin bed layer for later use.
Resin adsorption:
the feed liquid is subjected to necessary filtration pretreatment before being loaded onto a column for adsorption so as to remove solid impurities in the feed liquid and prevent the blockage of resin pore channels and the influence on the resin adsorption effect. The adsorption process generally adopts a positive column passing mode, the adsorption flow rate is generally recommended to be controlled at 1BV/h, and the adsorption state of the resin is determined by detecting the content of the target substance in the oral liquid.
And (3) water washing after adsorption:
after the resin adsorption is finished, the resin column bed is cleaned by using deionized water to pass through the column in a forward direction, the cleaning flow rate is generally controlled at 2BV/h, and the cleaning is carried out for 2h, so as to remove the residual feed liquid and part of water-soluble impurities in the column bed.
Resin analysis:
after the water washing is finished, according to the process design requirements, the resin is subjected to column chromatography by adopting a certain concentration and a certain amount of solvent (such as ethanol, methanol, acetone and the like). It should be noted that the resolving solution is a pure acetone solution.
Resin regeneration treatment:
(1) regeneration of alkali
Heating 4% sodium hydroxide solution to 85 deg.C, passing through the column in forward direction, and performing alkali regeneration treatment on the resin at flow rate of 1BV/h for about 1.5 h. After the regeneration treatment of the thermokalite is finished, the column is positively cleaned by deionized water, the cleaning flow rate is 3BV/h, and the pH value of the outlet liquid is less than or equal to 10.
(2) Acid regeneration
After the alkali regeneration and the water washing are finished, the forward column passing treatment is carried out by using 4 percent hydrochloric acid solution, the treatment flow rate is controlled to be 2BV/h, and the treatment time is about 1.5 h. After the acid regeneration treatment is finished, the column is positively cleaned by deionized water, the cleaning flow rate is 3BV/h, and the pH value of the outlet liquid is more than or equal to 5.
Comparative example 1
Chinese invention patent, application number: CN201310731832.6, publication No.: CN103720913B, which discloses a method for extracting tea polyphenol from tea by combining metal ion complexation precipitation and column chromatography, as described in the specification:
"a method for extracting tea polyphenol from tea by combining metal ion complexing precipitation and column chromatography, which comprises the following steps:
(1) raw material purchasing and detection
The tea raw material is purchased from the farmer market of Anhui fertile tea, and the content of tea polyphenol in the batch of tea is detected to be 25.11 percent according to the method of GB/T8313-;
(2) leaching tea raw materials 500g, pulverizing to 30 mesh, adding deionized water, performing ultrasonic leaching at 90 deg.C, stirring, refluxing for extraction for 30 min/time, leaching for 2 times (first 6000g deionized water, second 5000g deionized water), and filtering to obtain tea leaching solution;
(3) adding 20% ZnCl2 solution into the extractive solution according to the mass ratio of ZnCl to tea polyphenol of 2: 1, adjusting pH to 6.5 with 10% sodium bicarbonate solution, precipitating for 60min, centrifuging, and separating to obtain precipitate;
(4) acid hydrolysis
Fully dissolving the precipitate obtained in the step (3) by using 4mol/L hydrochloric acid to obtain tea polyphenol acid hydrolysate;
(5) extraction of
Adding ethyl acetate as extractant into acidolysis solution at volume ratio of 1:1, extracting at 50 deg.C for 3 times (each time for 30 min), and mixing ethyl acetate phases;
(6) concentrating
Adding ethyl acetate phase into a concentration tank, concentrating under reduced pressure at 60 deg.C, and recovering ethyl acetate to obtain crude extract of tea polyphenols;
(7) column chromatography
Selecting polyamide resin as a column filler, firstly soaking and activating the polyamide resin with 80% ethanol for one day, filling the polyamide resin into a column by a wet method, and washing the chromatographic column with weak acid solution to enable the chromatographic column to be in a weak acid environment; dissolving the crude extract of tea polyphenol with 1 time (g/ml) of deionized water, eluting with deionized water to colorless, eluting with 80% ethanol, vacuum concentrating the eluate, and vacuum drying to obtain tea polyphenol product with purity of 98.3% and extraction rate of 70.2%.
Comparative example 2
Chinese invention patent, application number: CN201410684591.9, publication No.: CN105693780A, discloses a method for extracting tea polyphenol, as the instruction of which is as follows:
"this embodiment provides a method for extracting tea polyphenols, which includes the following steps:
(1) coarse extraction: putting the green tea leaves after sieving and impurity removal and an ethanol solution which is 18 times of the green tea leaves and is at 55 ℃ into an extraction container, wherein the extraction container is a stainless steel cylinder with the diameter of 20 cm and the height of 40 cm; cutting and crushing the green tea leaves by using an inner blade and an outer blade, and maintaining the inner blade and the outer blade at an interval of 0.5 mm to 1.0 mm while the inner blade is at a rate of 1.5 × 104Cutting and stirring the green tea leaves in the extraction container at a speed of rpm around the center thereof to form crushed green tea leaves with a particle size of 40-60 meshes, and generating a vortex negative pressure of 0.4MPa to allow tea polyphenols to rapidly exude from the cells of the crushed green tea leaves and to be uniformly dispersed in the organic solvent; filtering to obtain tea polyphenol coarse extract;
(2) fine extraction: concentrating the crude tea polyphenol extracting solution under reduced pressure to obtain a tea polyphenol concentrated solution; diluting the tea polyphenol concentrated solution with distilled water to the concentration of 4.03 mg/mL; flowing the diluted tea polyphenol concentrated solution into XDA-1 macroporous resin chromatographic column (1.5 × 30cm) at a speed of 2.0 mL/min; eluting the XDA-1 macroporous resin chromatographic column with distilled water until the effluent is nearly colorless, and eluting with 70mL 80% ethanol at an elution rate of 1.4mL/min to obtain tea polyphenol ethanol-water eluate; and (3) concentrating the tea polyphenol alcohol-water eluent under reduced pressure, and drying to obtain a tea polyphenol finished product.
Comparative example 3
Chinese invention patent, application number: CN201310683801.8, publication No.: CN103704421B, disclosing one, as described in the specification:
the embodiment discloses a process for extracting tea polyphenol by ultrasonic supercritical combined extraction, which comprises the following steps:
1) drying fresh tea leaves to form dry tea leaves, selecting selected tea leaves, primarily crushing the residual tea dust to 60 meshes, mixing 5kg of tea dust with 50kg of hot water, and fully homogenizing in a vacuum high-shear homogenizer to obtain water paste slurry, wherein the water paste slurry is heated to 40 ℃ to improve the leaching rate.
2) Performing high-power microwave blasting treatment on the water paste slurry, wherein the microwave has high frequency and volatility and can break the cells of the tea by acting on polar molecules in the tea cells; the microwave adopts a high-power microwave generator, the working power is 800W, and the microwave time is 6 min.
3) High-power density ultrasonic treatment, mechanical crushing function of ultrasonic waves and generated cavitation effect are carried out on the water paste pulp, the cell walls of tea leaves are further damaged, in order to guarantee the effect, 18MHz and 20MHz sound fields are adopted for carrying out reverberation ultrasonic field treatment, the ultrasonic power is 1KW, the treatment time is 6min, so far, the tea leaves subjected to microwave and ultrasonic treatment are seriously damaged, and intracellular tea polyphenol components flow into hot water.
4) In order to obtain better tea polyphenol component and ensure the extraction rate of tea polyphenol, the paste is made into pasteAfter cooling, supercritical CO is utilized2Extracting tea polyphenols and removing caffeine, wherein the supercritical extraction process is carried out at 50 deg.C and 25MPa for 1 hr.
5) Concentrating the obtained solution containing a large amount of tea polyphenol by using a biological membrane system, and then spraying in a drying chamber.
Comparative example 4
Chinese invention patent, application number: CN201410838878.2, publication No.: CN104688935B, disclosing one, as described in the specification:
the fresh tea leaves in the embodiment are the narcissus tea in Zhangjing city, Fujian province, the content of tea polyphenol in the narcissus tea is 1.59%, and the specific steps of tea polyphenol extraction are as follows.
(1) And fresh leaves are collected: selecting fresh leaves of the Zhangping narcissus tea, picking, and collecting medium-open to large-open and bud-standing 3-4 leaf tips.
(2) Spreading and drying the fresh tea leaves on a clean appliance for 13-15h, preferably 15h, with the thickness of 10-15 cm; spreading and airing at 25-30 ℃.
(3) And enzyme deactivation: and (3) heating the spread and dried tea leaves in a microwave oven for 4min, wherein the output power of the microwave oven is 250-350W, and the optimal output power is 300W.
(4) Pulping: beating the heated tea leaves into pulp, adding normal-temperature purified water which is 10 times of the weight of the fresh tea leaves into a pulping machine, and setting the rotating speed of the pulping machine to 5200 r/min.
(5) And soaking: the slurry is held in a stainless steel barrel and soaked at normal temperature for 30 min.
(6) And squeezing: filtering the juice with a 300-mesh filter screen, and squeezing the filter residue with a filter press; adding 10 times of normal temperature purified water into the residue after squeezing and squeezing, stirring and soaking for 30min, and squeezing to obtain juice.
(7) And filtering: mixing the pulped filtrate and the juice obtained by squeezing the filter residue twice, and filtering with filter paper with the aperture of 1 mu m to obtain the crude tea polyphenol extracting solution.
(8) And high-speed centrifugation: and (3) centrifuging the crude extract by using a butterfly centrifuge at the rotating speed of 5500r/min to remove macroscopic granular impurities in the crude extract of the tea polyphenol.
(9) And fine filtering: selecting a melt-blown filter element with the aperture of 5 mu m to filter the tea polyphenol coarse extract after high-speed centrifugation, and further removing impurities in the tea polyphenol coarse extract.
(10) And ultrafiltration membrane filtration: filtering the fine-filtered filtrate by using an ultrafiltration membrane made of polyvinyl chloride and having a molecular weight cutoff of 10 ten thousand daltons, and controlling the temperature of the filtrate to be 40 +/-2 ℃ in the filtering process.
(11) Concentrating a reverse osmosis membrane: and concentrating the filtrate after ultrafiltration membrane treatment by using a reverse osmosis membrane until the concentration is 2%.
(12) Lignocellulose chromatography; selecting fir sawdust subjected to acid-base pretreatment as a column chromatography filler, adsorbing a concentrated solution obtained after concentration by a reverse osmosis membrane, eluting with purified water, and collecting eluates of different components.
The acid-base pretreatment process of the cedar wood chips comprises the following specific steps: placing Chinese fir chips on an enamel tray, baking for 4h in an oven at 105 ℃, then crushing by using a sample grinder, sieving by using a 0.45mm sieve, placing the undersize powder in a glass cylinder, adding 0.1N sodium hydroxide solution with twice volume, soaking for 7 days, taking out, filtering by using gauze, and washing by using distilled water until an eluent is colorless; putting the glass jar back, adding 0.1N hydrochloric acid with twice volume for soaking overnight, and washing with distilled water until the pH value is neutral; and then 90% ethanol is used for leaching until the mixture is colorless, and finally distilled water is used for washing the ethanol, and water is removed by vacuum filtration.
(13) And (3) spray drying: and (3) carrying out spray drying on the eluent with different components to obtain powder, thus obtaining catechin powders with different specifications.
Comparative example 5
Chinese invention patent, application number: CN201810334647.6, publication No.: CN108272695B, which discloses a method for extracting tea polyphenol for cosmetics, the specification of which is as follows:
"A method for extracting tea polyphenols for cosmetic comprises the following steps:
s1: raw material treatment: drying and crushing tea leaves into 80 meshes, adding distilled water as a solvent, fully homogenizing in a vacuum high-shear homogenizer to obtain water paste slurry, heating in a water bath to control the temperature of the water paste slurry to be 70 ℃, adding 10% ethanol into the water paste slurry, stirring at the speed of 260r/min for 30min, standing and cooling for 1h to obtain slurry a, and extracting the slurry a with a tetrahydrofuran solvent to obtain slurry b; the using amount ratio of the tea leaves to the distilled water is 1: 13; the dosage ratio of the tea leaves to the ethanol is 1: 0.5;
s2: ultrasonic treatment: carrying out ultrasonic treatment on the slurry b, wherein the frequency of the ultrasonic is 15-18KHz, and the treatment time is 15min to obtain slurry c;
s3: supercritical CO2And (3) extraction: subjecting the slurry c treated in step S2 to supercritical CO2Extraction in CO2Adding CO to the fluid2The fluid dosage of 17 percent of methanol, ethyl acetate and polysorbate is controlled, the extraction pressure is 22MPa, the extraction temperature is 45 ℃, and CO is controlled2The flow is 25L/h, the extraction time is 3h, a crude tea polyphenol product A is obtained, the crude tea polyphenol product A is separated from the pulp, the separation pressure is 5.5Mpa, and the separation temperature is 35 ℃; the residual slurry adopts supercritical CO again2Extraction in CO2Adding CO to the fluid2Acetone and methanol with 15% of fluid consumption, controlling extraction pressure at 22MPa, extraction temperature at 50 deg.C, and CO2The flow is 20L/h, the extraction time is 3h, a tea polyphenol crude product B is obtained, the tea polyphenol crude product B is separated from the pulp, the separation pressure is 4Mpa, and the separation temperature is 40 ℃; the weight ratio of the methanol to the ethyl acetate to the polysorbate is 2: 2.5: 2.2; the weight ratio of acetone to methanol is 1.2: 0.5;
s4: and (3) purification: mixing the obtained tea polyphenol crude product A and tea polyphenol crude product B, adding acetic acid, adjusting the pH value to 3.5, and then separating and purifying to obtain high-purity tea polyphenol; the concentration of the acetic acid is 22 percent, and the dosage of the acetic acid is 15 percent of the total amount of the crude tea polyphenol product.
Example 2
The tea polyphenols prepared in example 1 and the tea polyphenols prepared in comparative examples 1 to 5 (it is necessary to say that the tea leaves in comparative examples 1 to 5 are replaced with the tea leaves of this application for comparison) were selected and analyzed for the purity of the tea polyphenols (refer to GB/T8313-, 2016(2):257-261.).
As shown in table 3, the process of the present application has high indexes such as the extraction purity and extraction rate of tea polyphenols, and the clearance rate of DPPH free radicals, and thus, significant differences are reflected. Specifically, in comparative example 1, the original literature describes that the extraction purity and extraction rate are 98.3% and 70.2%, and it is noted that the calculation method of the extraction purity and extraction rate is different from that of the present application, in which the extraction purity and extraction rate of tea polyphenol of comparative example 1 are measured according to the method set forth in the present application; in addition, because the process of the method needs to adopt 90 ℃ ultrasonic leaching, the damage to tea polyphenol is large, and the subsequent use of zinc chloride is easy to cause residues. In comparative example 2, the originally recorded extraction purity and extraction rate were lower than those of example 1, and in comparative example 2, only column extraction was used, which severely affected the purity of tea polyphenols, and the high temperature from high speed rotary cutting also affected the extraction rate of tea polyphenols. In comparative example 3, the extraction process adopts a hot water mode, high-power microwave treatment is needed, the extraction rate of the tea polyphenol is influenced, and although a biological membrane is selected for filtration subsequently, the cost is higher. Comparative example 4 was similar to comparative example 5 in that the actual extraction purity, extraction yield and removal rate of DPPH radicals were low.
TABLE 3 alignment assay
While the invention has been described in further detail in connection with specific embodiments thereof, it will be understood that the invention is not limited thereto, and that various other modifications and substitutions may be made by those skilled in the art without departing from the spirit of the invention, which should be considered to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A method for extracting tea polyphenols for cosmetic comprises the following steps:
(1) pretreatment: preparing tea leaves, removing impurities on the surfaces of the tea leaves, cleaning and airing;
(2) polyvinyl alcohol treatment: transferring the tea leaves pretreated in the step (1) into a reaction tank, adding a polyvinyl alcohol solution for soaking, and washing with clear water after soaking;
(3) drying treatment: transferring the tea leaves treated by the polyvinyl alcohol in the step (2) into a low-temperature drying oven for drying;
(4) and (3) crushing treatment: selecting the tea leaves dried in the step (3), and transferring the tea leaves to a crusher for crushing;
(5) and (3) coarse extraction treatment: selecting the tea leaves crushed in the step (4), transferring the tea leaves into a reaction kettle, adding enzyme liquid, performing enzymolysis reaction, and centrifuging to recover clear liquid;
(6) fine extraction treatment: selecting the clear liquid obtained after the crude extraction in the step (5), transferring the clear liquid into a supercritical carbon dioxide extraction device, and recovering tea polyphenol slurry;
(7) secondary extraction treatment: selecting the tea polyphenol slurry after fine extraction in the step (6), selecting macroporous adsorption resin for impurity adsorption, and recovering effluent liquid;
(8) and (3) freeze drying treatment: and (4) selecting the effluent liquid obtained after the secondary extraction treatment in the step (7), conveying the effluent liquid into a vacuum freeze dryer, and pulverizing to obtain the powder.
2. The method of extracting tea polyphenol for cosmetics according to claim 1, characterized in that:
the variety of the tea in the step (1) is Meng Hai big leaf tea;
the impurities on the surface of the tea in the step (1) comprise soil particles, stone particles, dust and silt, and the impurities are removed by adopting a winnowing machine for screening; wherein the average wind speed of the air supply outlet of the air separator is 0.90m3(s), wherein the internal air pressure of the air separator is 300Pa, and the air separator; wherein before the tea leaves are loaded into the winnowing machine, a plurality of tea leaves are connected with the same tea stem for manual separation;
the cleaning mode in the step (1) is to soak the tea leaves by adopting warm water, the soaking time is controlled to be 20min, the temperature of the warm water is controlled to be 15 ℃, meanwhile, a stirrer is adopted to stir the soaked tea leaves, and the rotating speed of blades of the stirrer is controlled to be 20 r/min;
the drying mode in the step (1) is that the cleaned tea leaves are placed on a bamboo sieve and are naturally dried in the shade or dried by a fan, the time for naturally drying the tea leaves or the dried tea leaves by the fan is controlled within 4 hours, and the temperature of the shade is controlled within 20 ℃ during naturally drying or drying by the fan.
3. The method of extracting tea polyphenol for cosmetics according to claim 1, characterized in that:
the mass concentration of the polyvinyl alcohol solution in the step (2) is 10 percent;
controlling the temperature of the polyvinyl alcohol solution in the step (2) to be 25 ℃;
the soaking time of the polyvinyl alcohol solution in the step (2) is controlled to be 60 min;
and (3) the clean water in the step (2) is deionized water.
4. The method of extracting tea polyphenol for cosmetics according to claim 1, characterized in that:
the low-temperature drying box in the step (3) is a blast type drying box;
the drying temperature in the step (3) is 40 ℃;
the drying time in the step (3) is 1 h.
5. The method of extracting tea polyphenol for cosmetics according to claim 1, characterized in that:
the pulverizer in the step (4) is an airflow pulverizer;
controlling the working medium pressure of the pulverizer in the step (4) to be 0.4 MPa;
the average particle size of the crushed tea leaves in the step (4) is controlled to be 300 meshes.
6. The method of extracting tea polyphenol for cosmetics according to claim 1, characterized in that:
in the step (5), the enzyme solution is an aqueous solution containing cellulase, amylase, catalase and elastase, wherein the mass concentration of the enzyme solution is 3mg/mL, and the dosage ratio of the cellulase, the amylase, the catalase and the elastase is 1: 5: 3: 6;
the temperature of the enzymolysis reaction in the step (5) is 37 ℃.
7. The method of extracting tea polyphenol for cosmetics according to claim 6, characterized in that:
the centrifugal equipment in the step (5) is an ultracentrifuge;
the centrifugal force of the centrifugation in the step (5) is 100000 Xg;
the centrifugation time in the step (5) is 30 min;
the temperature of the centrifugation in the step (5) was 4 ℃.
8. The method of extracting tea polyphenol for cosmetics according to claim 1, characterized in that:
the model of the supercritical carbon dioxide extraction equipment in the step (6) is HA121-50-01, and the manufacturer is Jiangsu Nantong Huaan supercritical extraction company Limited;
the pressure of the supercritical carbon dioxide extraction in the step (6) is 21 MPa;
the temperature of the supercritical carbon dioxide extraction in the step (6) is 43 ℃;
the time of supercritical carbon dioxide extraction in step (6) is 20 min.
9. The method of extracting tea polyphenol for cosmetics according to claim 8, characterized in that:
adding an auxiliary agent into the carbon dioxide fluid of the supercritical carbon dioxide in the step (6), wherein the auxiliary agent is a mixture of ethyl acetate, propane and isopropyl ether, and the mass ratio of the ethyl acetate to the propane to the isopropyl ether is 3: 2: 2.
10. the method of extracting tea polyphenol for cosmetics according to claim 1, characterized in that:
the sample loading flow rate of the macroporous adsorption resin in the step (7) is 1 BV/h;
the model of the macroporous adsorption resin in the step (7) is LX-8, which is purchased from Xian lan Xiao science and technology New materials GmbH.
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Application publication date: 20210629 |