CN101235025A - Method for preparing theaflavin - Google Patents
Method for preparing theaflavin Download PDFInfo
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- CN101235025A CN101235025A CNA200810052355XA CN200810052355A CN101235025A CN 101235025 A CN101235025 A CN 101235025A CN A200810052355X A CNA200810052355X A CN A200810052355XA CN 200810052355 A CN200810052355 A CN 200810052355A CN 101235025 A CN101235025 A CN 101235025A
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- theoflavin
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- theaflavine
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Abstract
A preparation method of theaflavine belongs to agricultural product processing field, which relates to tea comprehensive processing. The invention resolves the problem of prior art as high cost in theaflavine preparation. The technical scheme comprises breaking fresh tea at low temperature, adding biological catalyst as plant leave juice, controlling the pH value of reaction liquid in the range of 4.0 to 6.0, feeding air at 25-50D EG C, mixing and reacting for 20-60min, separating solid and liquid after the reaction, feeding protecting agent into supernatant, concentrating at vacuum, directly atomizing, freezing and drying to obtain theaflavine product, or adding 95% alcohol of 1-3 powered volumes into supernatant, mixing for 20-40min, treating centrifugally to obtain supernatant and deposits, purifying the supernatant via macroporous adsorption resin, adding protecting agent, concentrating at vacuum, atomizing, freezing and drying to obtain theaflavine product. The preparation method of theaflavine confirms the stability of theaflavine and reduces production cost.
Description
One, technical field
The invention belongs to the processing of farm products field, relate to the tealeaves deep processing, particularly a kind of preparation method of theoflavin.
Two, background technology
At present, theoflavin is widely used in every field such as medicine, healthcare products, foodstuff additive because of it has higher resistance of oxidation.Be that tea-polyphenol in the polyphenol oxidase catalyzed tealeaves that utilizes in the tealeaves is transformed in the theoflavin production.Cost an arm and a leg owing to obtain pure product polyphenoloxidase, so enzyme is the key substance of producing theoflavin.Polyphenoloxidase content in the tealeaves is lower, directly utilizes the polyphenoloxidase in the tealeaves, has limited the production yield of theoflavin.
On July 21st, 1993 by the Decree of Patent Office of China a kind of " tea pigment and the mode of production thereof ", application number is 93110414.9, is characterized in directly utilizing using tealeaves, a kind of tea pigment based on theabrownin is produced in strong oxidation under high temperature highly basic condition.
On June 30th, 2004 by the Decree of Patent Office of China a kind of the method for high-purity theaflavin " immobile polyphenol oxidase catalyzed high-purity tea polyphenol produce ", the patent No. is ZL 02136982.8.Mays in 2005 25 door bolt by the Decree of Patent Office of China " a kind of composition that contains theoflavin and derivative thereof, with and preparation and purposes ", application number is 200310108715.0.
On May 25th, 2005 by the Decree of Patent Office of China " a kind of composition that contains theoflavin and derivative thereof, with and preparation and purposes ", application number is 200310108715.0.Be characterized in providing a kind of composition that contains multiple materials such as phosphatide, cholesterol.
On October 5th, 2005 by the Decree of Patent Office of China a kind of " high-active tawny agent and production method thereof ", the patent No. is ZL 00112536.2, its characteristics are to utilize the enzyme system of Fresh Folium Camelliae sinensis itself, under preferable oxypolymerization condition, make the tea leaf extract-tea-polyphenol that adds or the tea-polyphenol oxypolymerization in the expressed slag of the Fresh Folium Camelliae sinensis juice own become tea pigment based on theoflavin, thearubigins.
On September 27th, 2006 by the Decree of Patent Office of China " from tealeaves, extracting the method for tea-polyphenol, theanine, tea polysaccharide, theoflavin ", the patent No. is ZL 200610055145.7.Be characterized in adopting various technical processes to extract materials such as the tea-polyphenol in the tealeaves, theanine, tea polysaccharide and theoflavin respectively.
On December 13rd, 2006 by the Decree of Patent Office of China " method for extracting theaflavin ", the patent No. is ZL200510075693.1, its characteristics are for adding Fresh Folium Camelliae sinensis the water mill slurry after kneading, react oxidation then and obtain containing the solution of theoflavin, obtain centrifugate by centrifugal slagging-off, centrifugate obtains filtrate and adopts solvent extration or membrane separation process to handle to obtain theoflavin behind ceramic membrane ultrafitration.
March 14 in 2007 were fastened by the Decree of Patent Office of China " a kind of method of producing tea pigment " with a bolt or latch, the patent No. is ZL 200310112656.4, its characteristics be the enzyme that utilizes the enzyme of tealeaves itself to add or do not add to buy from market together the oxidized teas polyphenol generate the method for tea pigment.
Because pure product polyphenoloxidase costs an arm and a leg, polyphenoloxidase is all taken from tealeaves in the above patent, and the content of polyphenoloxidase is lower in the tealeaves, has limited biocatalysis efficient.Therefore, seeking to improve biocatalysis efficient by adding the method for cheap enzyme, is to improve the theoflavin yield, reduces the effective way of theoflavin production cost.Simultaneously, help the comprehensive utilization of resource, this is the main direction of this area research.
Three, summary of the invention
The production cost problem of higher that exists in the method at above-mentioned production theoflavin the invention provides and a kind ofly improves biocatalysis efficient by increasing the method that agricultural byproducts prepare theoflavin that adds of filling out the cheapness that contains polyphenoloxidase, reduces production costs.
Its main technical schemes: be to elect additional member plant leaf juice as biological catalyst; in the theoflavin preparation process; add biological catalyst---plant leaf juice on the one hand; improve catalytic efficiency; on the other hand; add protective material in the separation and purification process, carry out atomizing freeze drying and make theoflavin, concrete grammar is as follows:
(1) pre-treatment of raw material
With Fresh Folium Camelliae sinensis is to be placed on shady and cool dry place after raw material is removed impurity, cleaning, pulverizes.
(2) preparation of reaction solution
The above-mentioned raw material that crushes is encased in the reactor, is 1: 0.2～1 ratio according to Fresh Folium Camelliae sinensis than plant leaf juice weight ratio, adds plant leaf juice, is prepared into reaction solution.
(3) biocatalytic reaction prepares theoflavin
1) temperature is 25 ℃～50 ℃ in reaction process, and the pH value is 4.0-6.0, per minute unit volume reaction solution bubbling air 0.5～2 unit volume, and the stirring reaction time is 20～60 minutes;
2) after reaction finishes, carry out solid-liquid separation, in supernatant liquor, add protective material, by directly carrying out atomizing freeze drying behind the vacuum concentration, obtain the theoflavin goods again; Or in supernatant liquor, add 95% ethanol of 1-3 times of volume, stirred 20-40 minute, centrifugal must supernatant liquor and precipitation; supernatant liquor is obtained theoflavin solution after by macroporous adsorbent resin, add protective material, vacuum concentration again; after atomizing freeze drying obtains the theoflavin highly finished product.
Need to prove plant leaf juice, be selected from the leaf juice of plants such as hawthorn, persimmon, aloe, blueberry or lichee.
In addition, protective material is selected from vitamins C, sodium bisulfite or V-Brite B etc. in the separation and Extraction process.
Beneficial effect:
1. the leaf juice of electing hawthorn, persimmon, aloe, blueberry and the lichee of the cheapness that contains polyphenoloxidase additional member is biological catalyst.Make polyphenoloxidase in the reaction system except that from the tealeaves, added the agricultural byproducts that contain polyphenoloxidase again, improved biocatalysis efficient on the one hand, reduce the theoflavin production cost, make full use of the natural resources on the other hand.
2. owing to add antioxidant (vitamins C, sodium bisulfite or V-Brite B) in process of production, guaranteed the stability of theoflavin.
3. adopt the atomizing freeze drying technology, it is stable to help product, isolated with air in the refrigerating process, can prevent oxidation, has improved quality product.
Four, description of drawings
Fig. 1: be theoflavin preparation technology schema of the present invention.
Five, embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1:
The Fresh Folium Camelliae sinensis through precooling (the geographic tealeaves of Zhejiang balcony) 5kg with the aquatic foods harvesting, drop in the reactor after being crushed to 10 orders, add the pure juice of 2.5kg hawthorn leaf, the pH value that makes reaction solution is 5.0, per minute unit volume reaction solution bubbling air 1 unit volume, stirring reaction solid-liquid separation after 40 minutes under 30 ℃ of conditions, 95% ethanol that in liquid phase, adds 3 times of volumes (supernatant liquor), stirred 20 minutes, centrifugal supernatant liquor and the precipitation of getting, supernatant liquor by the D101 macroporous adsorbent resin, is obtained theoflavin solution.Add the 0.75g vitamins C, behind vacuum concentration, carry out atomizing freeze drying and make finished product.Wherein theoflavin content is more than 65%.
Embodiment 2:
Fresh Folium Camelliae sinensis 5kg with the aquatic foods harvesting through precooling, drop in the reactor after being crushed to 15 orders, 1.0kg the pure juice of Howthorn Leaf, the pH value that makes reaction solution is 5.5, per minute unit volume reaction solution bubbling air 1 unit volume, stirring reaction is after 30 minutes under 40 ℃ of conditions, solid-liquid separation adds the 0.6g vitamins C, behind vacuum concentration in supernatant liquor, carry out atomizing freeze drying, obtain finished product.Wherein theoflavin content is more than 42%.
Embodiment 3:
Fresh Folium Camelliae sinensis 5kg with the aquatic foods harvesting through precooling, drop in the reactor after being crushed to 20 orders, add the pure juice of 5kg lichee leaf, the pH value that makes reaction solution is 4.0, per minute unit volume reaction solution bubbling air 1 unit volume, stirring reaction is after 60 minutes under 30 ℃ of conditions, and solid-liquid separation adds 95% ethanol of 2 times of volumes (supernatant liquor) in supernatant liquor, stirred 40 minutes, centrifugal supernatant liquor and the precipitation of getting by the D101 macroporous adsorbent resin, obtains theoflavin solution with supernatant liquor.Add the 1g vitamins C, behind vacuum concentration, carry out atomizing freeze drying, obtain finished product.Wherein theoflavin content is more than 61%.
Embodiment 4:
Fresh Folium Camelliae sinensis 5kg with the aquatic foods harvesting through precooling, drop in the reactor after being crushed to 18 orders, add the pure juice of 2kg aloe, the pH value that makes reaction solution is 6.0, per minute unit volume reaction solution bubbling air 2 unit volumes, the ventilation stirring reaction is after 40 minutes under 45 ℃ of conditions, and solid-liquid separation adds 95% ethanol of 3 times of volumes (supernatant liquor) in supernatant liquor, stirred 30 minutes, centrifugal supernatant liquor and the precipitation of getting by the D101 macroporous adsorbent resin, obtains theoflavin solution with supernatant liquor.Add the 0.7g vitamins C, behind vacuum concentration, carry out atomizing freeze drying, obtain finished product.Wherein theoflavin content is more than 48%.
Embodiment 5:
Fresh Folium Camelliae sinensis 5kg with the aquatic foods harvesting through precooling, drop in the reactor after being crushed to 15 orders, add the pure juice of 3kg blueberry leaf, the pH value that makes reaction solution is 5.0, per minute unit volume reaction solution bubbling air 0.5 unit volume, the ventilation stirring reaction is after 60 minutes under 25 ℃ of conditions, and solid-liquid separation adds 95% ethanol of 3 times of volumes (supernatant liquor) in supernatant liquor, stirred 35 minutes, centrifugal supernatant liquor and the precipitation of getting by the D101 macroporous adsorbent resin, obtains theoflavin solution with supernatant liquor.Add the 0.5g sodium bisulfite, behind vacuum concentration, carry out atomizing freeze drying, obtain finished product.Wherein theoflavin content is more than 53%.
Embodiment 6:
Fresh Folium Camelliae sinensis 5kg with the aquatic foods harvesting through precooling, drop in the reactor after being crushed to 20 orders, add the pure juice of 2kg persimmon leaf, the pH value that makes reaction solution is 5.0, per minute unit volume reaction solution bubbling air 2 unit volumes, the ventilation stirring reaction is after 50 minutes under 35 ℃ of conditions, and solid-liquid separation adds 95% ethanol of 3 times of volumes (supernatant liquor) in supernatant liquor, stirred 30 minutes, centrifugal supernatant liquor and the precipitation of getting by the D101 macroporous adsorbent resin, obtains theoflavin solution with supernatant liquor.Add the 0.6g sodium sulfite, behind vacuum concentration, carry out atomizing freeze drying, obtain finished product.Wherein theoflavin content is more than 55%.
Claims (3)
1. the preparation method of a theoflavin; it is characterized in that electing additional member plant leaf juice as biological catalyst; in the theoflavin preparation process; add biological catalyst---plant leaf juice on the one hand; improve catalytic efficiency, on the other hand, in the separation and purification process, add protective material; carry out atomizing freeze drying and make theoflavin, concrete grammar is as follows:
(1) pre-treatment of raw material
With Fresh Folium Camelliae sinensis is to be placed on shady and cool dry place after raw material is removed impurity, cleaning, pulverizes;
(2) preparation of reaction solution
The above-mentioned raw material that crushes is encased in the reactor, is 1: 0.2～1 ratio according to Fresh Folium Camelliae sinensis than plant leaf juice weight ratio, adds plant leaf juice, is prepared into reaction solution;
(3) biocatalytic reaction prepares theoflavin
1) temperature is 25 ℃～50 ℃ in reaction process, and the pH value is 4.0-6.0, per minute unit volume reaction solution bubbling air 0.5～2 unit volume, and the stirring reaction time is 20～60 minutes;
2) after reaction finishes, carry out solid-liquid separation, in supernatant liquor, add protective material, by directly carrying out atomizing freeze drying behind the vacuum concentration, obtain the theoflavin goods again; Or in supernatant liquor, add 95% ethanol of 1-3 times of volume, stirred 20-40 minute, centrifugal must supernatant liquor and precipitation; supernatant liquor is obtained theoflavin solution after by macroporous adsorbent resin, add protective material, vacuum concentration again; after atomizing freeze drying obtains the theoflavin highly finished product.
2. according to the preparation method of the described a kind of theoflavin of claim 1, it is characterized in that plant leaf juice, be selected from the leaf juice of hawthorn, persimmon, aloe, blueberry or lichee.
3. according to the preparation method of the described a kind of theoflavin of claim 1, it is characterized in that protective material is selected from vitamins C, sodium bisulfite or V-Brite B in the separation and Extraction process.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101886097A (en) * | 2010-06-18 | 2010-11-17 | 江苏德和生物科技有限公司 | Preparation process for high purity theaflavin and application thereof in preparing anti-influenza virus medicines |
| CN102827896A (en) * | 2012-09-14 | 2012-12-19 | 向华 | Method for extracting theaflavin and theanine from tea leaves |
| CN104450822A (en) * | 2014-12-19 | 2015-03-25 | 雅安太时生物科技有限公司 | Method for producing theaflavin from tea polyphenol production wastewater |
| CN104498448A (en) * | 2014-12-31 | 2015-04-08 | 湖南农业大学 | Tea polyphenol oxidase isozyme monomers PP01 and PP02 and preparation method thereof |
| CN112546136A (en) * | 2020-12-21 | 2021-03-26 | 江苏德和生物科技有限公司 | Theaflavin tablet for preventing dental caries and its production process |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101081844B (en) * | 2006-06-01 | 2011-08-17 | 北京工商大学 | Method for large-batch separating preparation of high-purity theaflavine monomer |
| CN101096693B (en) * | 2007-07-26 | 2010-04-21 | 桂林莱茵生物科技股份有限公司 | Method for preparing theaflavin and thearubigin from fresh green tea |
-
2008
- 2008-02-29 CN CN200810052355XA patent/CN101235025B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101886097A (en) * | 2010-06-18 | 2010-11-17 | 江苏德和生物科技有限公司 | Preparation process for high purity theaflavin and application thereof in preparing anti-influenza virus medicines |
| CN102827896A (en) * | 2012-09-14 | 2012-12-19 | 向华 | Method for extracting theaflavin and theanine from tea leaves |
| CN102827896B (en) * | 2012-09-14 | 2014-03-26 | 广州市一杰医药科技有限公司 | Method for extracting theaflavin and theanine from tea leaves |
| CN104450822A (en) * | 2014-12-19 | 2015-03-25 | 雅安太时生物科技有限公司 | Method for producing theaflavin from tea polyphenol production wastewater |
| CN104498448A (en) * | 2014-12-31 | 2015-04-08 | 湖南农业大学 | Tea polyphenol oxidase isozyme monomers PP01 and PP02 and preparation method thereof |
| CN104498448B (en) * | 2014-12-31 | 2016-04-06 | 湖南农业大学 | Tea leaf polyphenols oxydase isozyme monomer PP01 and PP02 and preparation method thereof |
| CN112546136A (en) * | 2020-12-21 | 2021-03-26 | 江苏德和生物科技有限公司 | Theaflavin tablet for preventing dental caries and its production process |
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Owner name: FUJIAN SEIAN FOOD + TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: TIANJIN UNIVERSITY OF SCIENCE + TECHNOLOGY Effective date: 20120109 |
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Effective date of registration: 20120109 Address after: 355400 agricultural science and Technology Park in Zhouning County in Fujian Province Patentee after: Fujian Seian Food & Technology Co., Ltd. Address before: 83, box 1038, Tianjin University of Science and Technology, 300222 South Hexi District Road, Tianjin, Dagu Patentee before: Tianjin University of Science & Technology |
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Effective date of registration: 20181115 Address after: 352106 No. 15, Shu Gang Road, Zhangwan Town, Jiaocheng District, Ningde, Fujian. Patentee after: FUJIAN XIANYANGYANG BIOTECHNOLOGY CO., LTD. Address before: 355400 Agricultural Science and Technology Park, Zhouning County, Fujian Province Patentee before: Fujian Seian Food & Technology Co., Ltd. |
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