CN111217865A - Method for preparing tea polyphenol by compound enzyme supercritical fluid extraction - Google Patents
Method for preparing tea polyphenol by compound enzyme supercritical fluid extraction Download PDFInfo
- Publication number
- CN111217865A CN111217865A CN201811404419.8A CN201811404419A CN111217865A CN 111217865 A CN111217865 A CN 111217865A CN 201811404419 A CN201811404419 A CN 201811404419A CN 111217865 A CN111217865 A CN 111217865A
- Authority
- CN
- China
- Prior art keywords
- pressure
- valve
- extraction
- tea
- tea polyphenol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Tea And Coffee (AREA)
Abstract
The invention relates to a preparation method for extracting tea polyphenol from black tea, in particular to a method of a complex enzyme supercritical fluid extraction technology. The processing steps comprise: drying black tea, pulverizing, adding cellulase and pectinase at a ratio of 3:4, and mixing. A certain mass of the mix was weighed into the extractor and the equipment was flushed repeatedly with CO2 to remove air. During operation, the valve and the gas cylinder valve are opened to admit gas, the high-pressure valve is started to boost pressure, the pressure reducing valve is adjusted when the pressure rises to a preset pressure, the separation pressure in the separator is adjusted, the blow-down valve is opened to be connected with the rotor flowmeter to measure the flow, and the CO2 flow in the extraction process is stabilized at a required operation condition by adjusting each valve, the valve is semi-closed, the valve is opened to carry out full-cycle flow operation, and the extraction liquid is extracted from the oil blow-down valve in the extraction process. Concentrating under reduced pressure, and drying to obtain tea polyphenols powder. The method has the advantages of rapidness, high efficiency, small using amount of solvent and the like, and has good reproducibility, and the extracted tea polyphenol has high purity. Safe operation and environmental protection.
Description
Technical Field
The invention relates to a preparation method for extracting tea polyphenol by complex enzyme supercritical fluid, belonging to the field of extraction of effective components of plants.
Background
Black tea is dry tender leaf or leaf bud of Camellia sinensis belonging to Camellia of Theaceae, and is distributed in tropical and subtropical regions, and mainly produced in the south of Yangtze river. A large number of researches show that polyphenol as a secondary metabolite has a decisive effect on the taste and the nutritional value of tea. Tea polyphenol is a main effective component in tea, has various biological activities of resisting tumor, reducing blood fat, resisting atherosclerosis, strengthening heart, resisting arrhythmia, resisting aging, resisting bacteria and the like, and a large number of reports show that the biological activities are related to the antioxidant effect of the tea.
Tea polyphenols, also known as "Yioling", "Wei-polyphenol" and "Fanghailing", are polyhydroxy compounds contained in tea leaves, abbreviated as "TP", whose main chemical components are complexes of catechins (flavanols), flavones, flavonols, anthocyanidins, phenolic acids, depside acids, polymeric phenols, etc. China has rich tea resources but low utilization rate. With the expansion of the application field of the effective components of tea such as tea polyphenol, caffeine and tea polysaccharide, the market demand at home and abroad is increasing day by day. Therefore, many researchers have been interested in extracting and separating effective components from waste tea leaves. The traditional extraction methods mainly comprise a solvent extraction method, an ion precipitation method, an ultrasonic extraction method, a supercritical fluid extraction method and the like, and the separation methods comprise a column chromatography method, a macroporous adsorption resin method, a high-speed counter-current chromatography method, a membrane separation method and the like. However, these methods all have the characteristics of large solvent consumption and high material cost.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing tea polyphenol, which has high efficiency and selectivity, simple and convenient operation, high yield and few byproducts and can be realized industrially.
The technical scheme of the invention is carried out according to the following steps:
a. drying black tea, pulverizing, adding cellulase and pectinase at a ratio of 3:4, pulverizing for the second time, sieving with 80 mesh sieve, and mixing;
b. weighing a certain mass of mixture, loading the mixture into an extractor, and repeatedly flushing equipment with CO2 to remove air;
c. during operation, firstly opening a valve and a gas cylinder valve to admit gas, then starting a high-pressure valve to boost pressure, adjusting a pressure reducing valve when the pressure is increased to a preset pressure, adjusting the separation pressure in a separator, then opening an emptying valve to be connected with a rotor flowmeter to measure the flow, and adjusting each valve to stabilize the extraction pressure, the separation pressure and the flow passing through CO2 in the extraction process at the required operation condition, semi-closing the valves, opening the valves to perform full-cycle flow operation, and extracting the extract from an oil drainage valve in the extraction process;
and d, concentrating the extract liquor under reduced pressure and drying to obtain tea polyphenol powder.
1. The method for extracting tea polyphenol from black tea by using the complex enzyme supercritical fluid extraction technology as claimed in claim 1, wherein the ratio of the cellulase to the pectinase in the step a is 3:4, and the material powder is smaller than 80 meshes.
2. The method for extracting tea polyphenol from black tea by the compound enzyme supercritical fluid extraction technology as claimed in claim 1, wherein the extraction conditions in the step c are as follows: the high-pressure pump is selected, and the three-plunger high-pressure pump can better meet the requirement of supercritical CO2 extraction industrialization. The extraction pressure is 7.38MPa, the extraction temperature is 31.05 ℃, and the entrainer selection solvent is chloroform.
The invention has the advantages that:
1. the invention adopts the compound enzyme to treat the raw materials, realizes the one-step completion of crushing and treatment, adopts the compound enzyme liquid with the main components of cellulase and pectinase to decompose cellulose, hemicellulose and pectin which form cell walls and intercellular substances in experiments, increases the diffusion area and improves the extraction rate of tea polyphenol.
2. The invention adopts Supercritical Fluid Extraction (SFE) which is a novel separation technology introduced into China in the 80 th of the 20 th century. Compared with the traditional extraction and separation method, the SFE has the greatest advantage that the SFE can extract and separate compounds with different polarities and different boiling points under the condition of near normal temperature and normal pressure; by changing the extraction pressure and temperature or adding proper entrainer, the solubility and selectivity of the extractant can be changed, and the extraction efficiency is improved.
The present invention will be further described with reference to specific embodiments, but the scope of the invention as claimed is not limited to the following embodiments.
The specific implementation mode is as follows:
example 1:
drying black tea, pulverizing, adding cellulase and pectinase at a ratio of 3:4, pulverizing for the second time, sieving with 80 mesh sieve, and mixing; weighing a certain mass of mixture, loading the mixture into an extractor, and repeatedly flushing equipment with CO2 to remove air; during operation, firstly opening a valve and a gas cylinder valve to admit gas, then starting a high-pressure valve to boost pressure, adjusting a pressure reducing valve when the pressure is increased to a preset pressure, adjusting the separation pressure in a separator, then opening an emptying valve to be connected with a rotor flowmeter to measure the flow, and adjusting each valve to stabilize the extraction pressure, the separation pressure and the flow passing through CO2 in the extraction process at the required operation condition, semi-closing the valves, opening the valves to perform full-cycle flow operation, and extracting the extract from an oil drainage valve in the extraction process; concentrating the extractive solution under reduced pressure, and drying to obtain tea polyphenols powder.
Example 2:
drying black tea, pulverizing, adding cellulase and pectinase at a ratio of 3:5, pulverizing for the second time, sieving with 80 mesh sieve, and mixing; weighing a certain mass of mixture, loading the mixture into an extractor, and repeatedly flushing equipment with CO2 to remove air; during operation, firstly opening a valve and a gas cylinder valve to admit gas, then starting a high-pressure valve to boost pressure, adjusting a pressure reducing valve when the pressure is increased to a preset pressure, adjusting the separation pressure in a separator, then opening an emptying valve to be connected with a rotor flowmeter to measure the flow, and adjusting each valve to stabilize the extraction pressure, the separation pressure and the flow passing through CO2 in the extraction process at the required operation condition, semi-closing the valves, opening the valves to perform full-cycle flow operation, and extracting the extract from an oil drainage valve in the extraction process; concentrating the extractive solution under reduced pressure, and drying to obtain tea polyphenols powder.
Example 3:
drying black tea, pulverizing, adding cellulase and pectinase at a ratio of 3:6, pulverizing again, sieving with 80 mesh sieve, and mixing; weighing a certain mass of mixture, loading the mixture into an extractor, and repeatedly flushing equipment with CO2 to remove air; during operation, firstly opening a valve and a gas cylinder valve to admit gas, then starting a high-pressure valve to boost pressure, adjusting a pressure reducing valve when the pressure is increased to a preset pressure, adjusting the separation pressure in a separator, then opening an emptying valve to be connected with a rotor flowmeter to measure the flow, and adjusting each valve to stabilize the extraction pressure, the separation pressure and the flow passing through CO2 in the extraction process at the required operation condition, semi-closing the valves, opening the valves to perform full-cycle flow operation, and extracting the extract from an oil drainage valve in the extraction process; concentrating the extractive solution under reduced pressure, and drying to obtain tea polyphenols powder.
Claims (3)
1. A preparation method for extracting tea polyphenol from black tea, in particular to a method of a complex enzyme supercritical fluid extraction technology. The method is characterized in that:
a. drying black tea, pulverizing, adding cellulase and pectinase at a ratio of 3:4, pulverizing for the second time, sieving with 80 mesh sieve, and mixing;
b. weighing a certain mass of mixture, loading the mixture into an extractor, and repeatedly flushing equipment with CO2 to remove air;
c. during operation, firstly opening a valve and a gas cylinder valve to admit gas, then starting a high-pressure valve to boost pressure, adjusting a pressure reducing valve when the pressure is increased to a preset pressure, adjusting the separation pressure in a separator, then opening an emptying valve to be connected with a rotor flowmeter to measure the flow, and adjusting each valve to stabilize the extraction pressure, the separation pressure and the flow passing through CO2 in the extraction process at the required operation condition, semi-closing the valves, opening the valves to perform full-cycle flow operation, and extracting the extract from an oil drainage valve in the extraction process;
and d, concentrating the extract liquor under reduced pressure and drying to obtain tea polyphenol powder.
2. The method for extracting tea polyphenol from black tea by using the complex enzyme supercritical fluid extraction technology as claimed in claim 1, wherein the ratio of the cellulase to the pectinase in the step a is 3:4, and the material powder is smaller than 80 meshes.
3. The method for extracting tea polyphenol from black tea by the compound enzyme supercritical fluid extraction technology as claimed in claim 1, wherein the extraction conditions in the step c are as follows: the high-pressure pump is selected, and the three-plunger high-pressure pump can better meet the requirement of supercritical CO2 extraction industrialization. The extraction pressure is 7.38MPa, the extraction temperature is 31.05 ℃, and the entrainer selection solvent is chloroform.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811404419.8A CN111217865A (en) | 2018-11-23 | 2018-11-23 | Method for preparing tea polyphenol by compound enzyme supercritical fluid extraction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811404419.8A CN111217865A (en) | 2018-11-23 | 2018-11-23 | Method for preparing tea polyphenol by compound enzyme supercritical fluid extraction |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111217865A true CN111217865A (en) | 2020-06-02 |
Family
ID=70808470
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811404419.8A Pending CN111217865A (en) | 2018-11-23 | 2018-11-23 | Method for preparing tea polyphenol by compound enzyme supercritical fluid extraction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111217865A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113041188A (en) * | 2021-03-18 | 2021-06-29 | 广州妙思生物科技有限公司 | Method for extracting tea polyphenol for cosmetics |
-
2018
- 2018-11-23 CN CN201811404419.8A patent/CN111217865A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113041188A (en) * | 2021-03-18 | 2021-06-29 | 广州妙思生物科技有限公司 | Method for extracting tea polyphenol for cosmetics |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109942380B (en) | Method for preparing cannabidiol by high-speed counter-current chromatography separation and purification | |
| CN102432582A (en) | Preparation method of proanthocyanidin | |
| CN101928639A (en) | Natural tea essence prepared by using tea and preparation method thereof | |
| CN101429222A (en) | Method for extracting mangiferin | |
| CN104523767B (en) | A kind of method for extracting Flavonoid substances in cacumen biotae | |
| CN101402657A (en) | Process for producing chestnut shell polyphenol | |
| CN101463027A (en) | Method for extracting and separating flavone and anthocyanidin from elder fruit | |
| CN103772339B (en) | A kind of method extracting NVP-XAA 723 from tealeaves tankage | |
| CN104045671A (en) | Method for extracting and purifying phlorizin in apple root-bark | |
| CN101402864A (en) | Method for producing oxidation resistant product from rosemary | |
| CN104771930B (en) | The Subcritical Water Extraction agent of polyphenols and extracting process in a kind of lotus solid waste | |
| CN107118253A (en) | The preparation method of Tea Saponin | |
| CN105985315A (en) | Method for extracting nicotine from tobacco waste | |
| CN111217865A (en) | Method for preparing tea polyphenol by compound enzyme supercritical fluid extraction | |
| CN104910223A (en) | Preparation method of oleuropein | |
| CN110590510B (en) | Preparation method of cannabidiol | |
| CN104450822A (en) | Method for producing theaflavin from tea polyphenol production wastewater | |
| CN109021042B (en) | Method for extracting high-purity oleuropein from olive leaves | |
| CN110922413A (en) | Extraction and separation method of glabridin | |
| CN104945450A (en) | Method for extracting stibene glucoside from vines of multiflower knotweeds | |
| CN107669716A (en) | The method that general flavone is extracted from desmodium | |
| CN114907191A (en) | Hemp impurity removal method | |
| CN111388550B (en) | Preparation method of anticancer active polyphenol of plums | |
| CN107375537A (en) | The preparation method of Tea Polyphenols in southwestern camellia | |
| CN112939744A (en) | Efficient extraction method of cannabidiol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20200602 |
|
| WD01 | Invention patent application deemed withdrawn after publication |