CN101691591A - Industrial preparation method of theaflavin - Google Patents
Industrial preparation method of theaflavin Download PDFInfo
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- CN101691591A CN101691591A CN200910153520A CN200910153520A CN101691591A CN 101691591 A CN101691591 A CN 101691591A CN 200910153520 A CN200910153520 A CN 200910153520A CN 200910153520 A CN200910153520 A CN 200910153520A CN 101691591 A CN101691591 A CN 101691591A
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Abstract
The invention relates to an industrial preparation method of theaflavin, which comprises the following steps: (1) preparing an ethyl acetate solution containing rich tea polyphenol; (2) respectively adding pulverized fresh tea leaves and the ethyl acetate solution into a oxidation-fermentation tank, orderly adding ethyl acetate and a buffering solution, introducing air at normal temperature, and stirring, oxidizing and fermenting to obtain the theaflavin ester-phase solution; (3) filtering the theaflavin ester-phase solution, concentrating and washing to remove impurities; (4) concentrating the water-phase solution, and spray-drying to obtain low-specification dry theaflavin powder; (5) concentrating the ester-phase solution to recycle ethyl acetate, and adding water so that the theaflavin is dissolved in the water; (6) centrifugally filtering the theaflavin water solution to obtain a pure theaflavin solution; (7) and concentrating the theaflavin solution, and spray-drying to obtain the dry theaflavin powder. The method of the invention simultaneously enhances the yield and the quality of the theaflavin, saves the energy and the man hours and reduces the emission of waste water.
Description
(1) technical field
The present invention relates to a kind of industrialization method of from tealeaves, producing theoflavin.
(2) background technology
In recent years, along with the theoflavin class in the modern medicine study discovery black tea has stronger biological activity, the superiority of its function and see broadness more in Application Areass such as natural drug, functional food and beverage, daily-use chemical industries, cause extraction theoflavin from black tea does not have cost performance economically, and the different for this reason methods of theoflavin that prepare are by appearing in the newspapers.Be following trend with external oxidation (enzymatic oxidn or chemical oxidation) Preparing Tea-polyphenol theoflavin especially wherein.Though seeking new enzyme source and immobilization technology thereof and new oxygenant is the vital task that the in-vitro simulated oxidation of tea-polyphenol prepares theoflavin, but this is an aerobic processes, and therefore " biliquid ferments mutually " provides new thinking for this process again to improving mass transfer and tunning.In addition, still relate to and prevent that theoflavin from not continued to be oxidized to theabrownin and to the separation and purification program of the complex and expensive of product, these have all restricted the scale production of theoflavin.
Chinese invention patent CN1699358 discloses a kind of extracting method of theoflavin, this method is that Fresh Folium Camelliae sinensis is added the water mill slurry after kneading, the oxidation of fermenting then obtains containing the solution of theoflavin, obtain centrifugate by centrifugal slagging-off, centrifugate gained filtrate behind ceramic membrane ultrafitration is adopted solvent extration or membrane separation process to handle and is obtained theoflavin.The extracting method technology of this theoflavin is simple, and cost is low, meets environmental protection requirement; product yield height; the content height, and can satisfy the needs of industries such as medicine, healthcare products, food by the different different series product of processing condition output content of control.
Chinese invention patent CN101235025 discloses a kind of preparation method of theoflavin, its technical scheme is with after the Fresh Folium Camelliae sinensis pulverize at low temperature, add biological catalyst such as plant leaf juice, the reaction solution pH value is in 4.0～6.0 scopes, bubbling air under 25 ℃～50 ℃ condition, stirring reaction 20～60 minutes.Reaction is carried out solid-liquid separation after finishing, and adds protective material in supernatant liquor, obtains the theoflavin goods by direct atomizing freeze drying behind the vacuum concentration again; Or in supernatant liquor, add 95% ethanol of 1～3 times of volume, and stirring 20～40 minutes, centrifugal supernatant liquor and precipitation by behind the purification with macroreticular resin, add protective material with supernatant liquor, and atomizing freeze drying behind the vacuum concentration obtains the theoflavin highly finished product.Preparation method of the present invention has guaranteed the stability of theoflavin, has reduced production cost.
Chinese invention patent CN101285081 provides a kind of enzyme that utilizes tealeaves self tea-polyphenol in the tealeaves to be prepared the novel process of theoflavin by bio-transformation.Its preparation process is: green tea is added the fermenting enzyme for preparing with fresh tea leaf in its after ethyl acetate extraction, feed under the pure oxygen and stir fermentation, then through separating, concentrate, wash, change molten, filtering, carry out vacuum lyophilization at last, pulverize, sieve, thereby obtain qualified theoflavin product.The theoflavin Product Green environmental protection that makes by this technology, steady quality, theoflavin content height, the yield height, cost is low, and because the pure ester phase oxidation fermentation that present method adopts, solved after traditional ester, water, the fermentation of slag mixed phase can't three phase separation problem, thereby can carry out the technology production of stable and controllable.
(3) summary of the invention
Technical problem to be solved by this invention is to provide that a kind of production technique is simple, process stabilization is controlled, production cost is relatively low, can make the industrialization preparation method of high-quality theoflavin.
A kind of industrialization preparation method of theoflavin comprises following sequential steps:
(1) by preparing the ethyl acetate solution that is rich in tea-polyphenol in the tealeaves;
(2) will pulverize the bright leaf of tea respectively and drop into the oxidative fermentation jar with the ethyl acetate solution that is rich in tea-polyphenol, add ethyl acetate and buffering solution successively, bubbling air stirred oxidative fermentation 30-50 minute under the normal temperature, obtain theoflavin ester phase solution, wherein the amount ratio of the bright leaf of tea, the ethyl acetate solution that is rich in tea-polyphenol, ethyl acetate, buffered soln is 800Kg: 600-900Kg: 15-25L: 1-2L;
(3) theoflavin ester phase solution is earlier removed tea grounds after filtration, concentrates the back again and washes assortedly with weak acid liquid or weak lye, washes and obtains aqueous phase solution and ester solution mutually after mixing;
(4) aqueous phase solution of step (3) concentrates the back spraying drying, obtains the theoflavin dry powder of low specification;
(5) the ester phase solution concentration of step (3) adds entry then and makes theoflavin change molten in water to reclaim ethyl acetate;
(6) the theoflavin aqueous solution that changes after molten carries out centrifuging, removes solid impurity, obtains purified theoflavin solution;
(7) the theoflavin solution concentration is arrived solid content 20-30%, spraying drying promptly obtains the theoflavin dry powder of purity more than 40% then.
Step of the present invention (1) can adopt method commonly known in the art to make, as Chinese patent CN101285081 disclosed method.The tea-polyphenol concentration that makes is generally 50-100mg/ml.
Preferably, the described buffered soln of step (2) is citric acid-Sodium phosphate dibasic buffer reagent.Ethyl acetate is as extraction solvent in the step (2), and damping fluid effect in the present invention is to regulate pH, and the pH scope of recommendation is 4.5～5.
Preferably, the described weak acid liquid of step (3) is a citric acid solution.
Preferably, the described weak lye of step (3) is sodium hydrogen carbonate solution or weakly alkaline Tris-HCL solution.
Preparation method of the present invention makes tea-polyphenol utilize the oxidase catalyzed tea-polyphenol of pulverizing the bright leaf self of tea in biliquid phase (water with ester mutually), solid phase, gas phase.Biliquid mutually in evenly bubbling air stir oxidative fermentation, guarantee the mildness and the stability of biological oxidation process.The tea-polyphenol of ester phase (matrix) constantly changes molten to aqueous phase in the oxidative fermentation process, after being rich in oxidasic aqueous phase to be theoflavin, constantly change again by catalyzed oxidation be dissolved in ester mutually in, cause biliquid is alternate in the reaction system response matrix and reaction product constantly to shift and reach running balance, make a spot of enzyme source bring into play its maximum catalytic efficiency.Meanwhile, impel this reaction system to be able to abundant conversion (transformation efficiency reaches more than 80%), and it is excessive effectively to control reaction, reduces the generation of theabrownin because the adding of ester phase increases the dissolved oxygen ability in this system.After oxidation is finished, extract synchronously, can obtain high-purity theaflavin product (content reaches more than 50%) once going on foot, yield can reach more than 50% (in the tea-polyphenol).Because preparation method of the present invention can finish in the equipment of producing tea-polyphenol, so simplified reparation technology and equipment, process stabilization is controlled, production cost is relatively low, is convenient to suitability for industrialized production in addition.
Beneficial effect of the present invention is:
1, utilizes the oxydase that self contains in the Fresh Folium Camelliae sinensis, without purifying or fixing, directly the catalysis tea-polyphenol is converted into theoflavin, has changed other technologies and need extract the enzyme source or utilize chemical oxidizing agent to produce the defective of the method for theoflavin, produces the highly purified theoflavin of pure natural;
2, adopt the bright leaf of tea-polyphenol liquid and tea to ferment and directly produced, changed the technology that adopts tea-polyphenol pulvis oxidative fermentation.Directly extract with tea-polyphenol feed liquid oxidative fermentation solvent, reduced the subsequent handling that the tea-polyphenol pulvis is produced, saved the energy and man-hour, reduced discharge of wastewater again, not only reduced production cost but also environmental protection, improved the yield and the quality of theoflavin simultaneously;
3, theoflavin is produced with tea-polyphenol and is produced and can carry out on same equipment, utilizes same set of device just to change processing condition and can produce theoflavin and two kinds of products of tea-polyphenol respectively, has improved usage ratio of equipment;
4, the oxygenation of tea-polyphenol among the preparation method, enzymatic oxidn and theoflavin extraction are carried out synchronously, have protected the activity of enzyme so on the one hand, and whole process mitigation, controlled makes the transformation efficiency height of tea-polyphenol; It is excessive to be difficult for reaction again.Only need after the fermentation ends ester is carried out impurity elimination mutually, concentrates, changes molten processing, can reach one and go on foot the purpose of producing the high-purity theaflavin product;
5, to adopt weak base or weakly acid soln to wash assorted, the environmental issue of having avoided use halohydrocarbon noxious solvents such as (as not chloroform, methylene dichloride) to bring.
(4) description of drawings
Fig. 1 is a preparation method's of the present invention process flow sheet.
(5) embodiment
The present invention is further illustrated below in conjunction with drawings and Examples, but protection scope of the present invention is not limited to this.
Embodiment 1
(1) obtains the ethyl acetate solution that 700kg is rich in the 80mg/ml tea-polyphenol by the prepared of extracting tea-polyphenol;
(2) 700kg being rich in the ethyl acetate solution of tea-polyphenol and the bright leaf of tea of 800kg pulverizing drops in the oxidative fermentation jar, citric acid-Sodium phosphate dibasic the buffer reagent that adds 20L ethyl acetate and 1.5L successively, under the normal temperature state, bubbling air stirred oxidative fermentation 30-40 minute, got theoflavin ester phase solution;
(3) theoflavin ester phase solution is earlier removed tea grounds after filtration, concentrates the back again and washes assortedly with sodium hydrogen carbonate solution, washes and obtains aqueous phase solution and ester solution mutually after mixing; The tea grounds oven dry, other deposits standby.
(4) aqueous phase solution of step (3) concentrates the back spraying drying, obtains the theoflavin dry powder of low specification;
(5) the ester phase solution concentration of step (3) adds entry then and makes theoflavin change molten in water to reclaim ethyl acetate;
(6) the theoflavin aqueous solution that changes after molten carries out centrifuging, removes solid impurity, obtains purified theoflavin solution;
(7) the theoflavin solution concentration is arrived solid content 20-30%, spraying drying promptly obtains the theoflavin power-product of high standard then.
Calculate after testing, the purity of theoflavin power-product is 55.6%, and yield is 54% (in tea-polyphenol).
Embodiment 2
(1) obtains the ethyl acetate solution that 800kg is rich in the 80mg/ml tea-polyphenol by the prepared of extracting tea-polyphenol;
(2) 800kg being rich in the ethyl acetate solution of tea-polyphenol and the bright leaf of tea of 800kg pulverizing drops in the oxidative fermentation jar, citric acid-Sodium phosphate dibasic the buffer reagent that adds 24L ethyl acetate and 1.8L successively, under the normal temperature state, bubbling air stirred oxidative fermentation 30-40 minute, got theoflavin ester phase solution;
(3) theoflavin ester phase solution is earlier removed tea grounds after filtration, concentrates the back again and washes assortedly with citric acid solution, washes and obtains aqueous phase solution and ester solution mutually after mixing; The tea grounds oven dry, other deposits standby.
(4) aqueous phase solution of step (3) concentrates the back spraying drying, obtains the theoflavin dry powder of low specification;
(5) the ester phase solution concentration of step (3) adds entry then and makes theoflavin change molten in water to reclaim ethyl acetate;
(6) the theoflavin aqueous solution that changes after molten carries out centrifuging, removes solid impurity, obtains purified theoflavin solution;
(7) the theoflavin solution concentration is arrived solid content 20-30%, spraying drying promptly obtains the theoflavin power-product of high standard then.
Calculate after testing, the purity of theoflavin power-product is 56.3%, and yield is 56% (in tea-polyphenol).
Claims (4)
1. the industrialization preparation method of a theoflavin is characterized in that comprising following sequential steps:
(1) by preparing the ethyl acetate solution that is rich in tea-polyphenol in the tealeaves;
(2) will pulverize the bright leaf of tea respectively and drop into the oxidative fermentation jar with the ethyl acetate solution that is rich in tea-polyphenol, add ethyl acetate and buffering solution successively, bubbling air stirred oxidative fermentation 30-50 minute under the normal temperature, obtain theoflavin ester phase solution, wherein the amount ratio of the bright leaf of tea, the ethyl acetate solution that is rich in tea-polyphenol, ethyl acetate, buffered soln is 800Kg: 600-900Kg: 15-25L: 1-2L;
(3) theoflavin ester phase solution is earlier removed tea grounds after filtration, concentrates the back again and washes assortedly with weak acid liquid or weak lye, washes and obtains aqueous phase solution and ester solution mutually after mixing;
(4) aqueous phase solution of step (3) concentrates the back spraying drying, obtains the theoflavin dry powder of low specification;
(5) the ester phase solution concentration of step (3) adds entry then and makes theoflavin change molten in water to reclaim ethyl acetate;
(6) the theoflavin aqueous solution that changes after molten carries out centrifuging, removes solid impurity, obtains purified theoflavin solution;
(7) the theoflavin solution concentration is arrived solid content 20-30%, spraying drying promptly obtains the theoflavin dry powder of purity more than 40% then.
2. according to the industrialization preparation method of the theoflavin of claim 1, it is characterized in that: the described buffered soln of step (2) is citric acid-Sodium phosphate dibasic buffer reagent.
3. according to the industrialization preparation method of the theoflavin of claim 1 or 2, it is characterized in that: the described weak acid liquid of step (3) is a citric acid solution.
4. according to the industrialization preparation method of the theoflavin of claim 1 or 2, it is characterized in that: the described weak lye of step (3) is sodium hydrogen carbonate solution or weakly alkaline Tris-HCL solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101535205A CN101691591B (en) | 2009-09-30 | 2009-09-30 | Industrial preparation method of theaflavin |
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| CN2009101535205A CN101691591B (en) | 2009-09-30 | 2009-09-30 | Industrial preparation method of theaflavin |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250980A (en) * | 2011-06-16 | 2011-11-23 | 中华全国供销合作总社杭州茶叶研究所 | Process for extracting theaflavin product |
| CN103694727A (en) * | 2013-12-11 | 2014-04-02 | 浙江茗皇天然食品开发有限公司 | Method for separating tea pigment from instant tea slagging waste liquid |
| 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 |
| CN105734090A (en) * | 2016-02-01 | 2016-07-06 | 中国人民解放军总后勤部军需装备研究所 | Theaflavin preparation method |
| CN109852646A (en) * | 2018-12-14 | 2019-06-07 | 成都华高生物制品有限公司 | A method of theaflavin is prepared using fresh tea leaf |
| CN110367355A (en) * | 2019-08-07 | 2019-10-25 | 云南茶农生物产业有限责任公司 | A kind of high content of theaflavins and protect fragrant instant black tea powder, preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1221178C (en) * | 2000-09-14 | 2005-10-05 | 赵剑 | High-active tawny agent and productive method thereof |
| CN1304586C (en) * | 2003-12-13 | 2007-03-14 | 无锡市世纪生物药业有限公司 | Method for preparing tea pigment |
| CN1289492C (en) * | 2005-06-15 | 2006-12-13 | 海南群力药业有限公司 | Method for extracting theaflavin |
| CN101285081B (en) * | 2008-04-08 | 2011-12-21 | 江苏德和生物科技有限公司 | New process for preparing theaflavine |
-
2009
- 2009-09-30 CN CN2009101535205A patent/CN101691591B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102250980A (en) * | 2011-06-16 | 2011-11-23 | 中华全国供销合作总社杭州茶叶研究所 | Process for extracting theaflavin product |
| CN103694727A (en) * | 2013-12-11 | 2014-04-02 | 浙江茗皇天然食品开发有限公司 | Method for separating tea pigment from instant tea slagging waste liquid |
| CN103694727B (en) * | 2013-12-11 | 2015-10-14 | 浙江茗皇天然食品开发有限公司 | A kind of method being separated tea pigment from instant tea deslagging waste liquid |
| 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 |
| CN105734090A (en) * | 2016-02-01 | 2016-07-06 | 中国人民解放军总后勤部军需装备研究所 | Theaflavin preparation method |
| CN109852646A (en) * | 2018-12-14 | 2019-06-07 | 成都华高生物制品有限公司 | A method of theaflavin is prepared using fresh tea leaf |
| CN110367355A (en) * | 2019-08-07 | 2019-10-25 | 云南茶农生物产业有限责任公司 | A kind of high content of theaflavins and protect fragrant instant black tea powder, preparation method thereof |
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| CN101691591B (en) | 2011-11-23 |
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