CN1626668A - Method for preparing tea pigment - Google Patents
Method for preparing tea pigment Download PDFInfo
- Publication number
- CN1626668A CN1626668A CN 200310112656 CN200310112656A CN1626668A CN 1626668 A CN1626668 A CN 1626668A CN 200310112656 CN200310112656 CN 200310112656 CN 200310112656 A CN200310112656 A CN 200310112656A CN 1626668 A CN1626668 A CN 1626668A
- Authority
- CN
- China
- Prior art keywords
- tea
- organic phase
- temperature
- tea pigment
- organic solvent
- 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.)
- Granted
Links
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
A process for preparing the tea pigment includes such steps as mashing fresh tea leaves, adding enzyme, adding them to the solution of theopolyphenol in organic solvent, adding acidic aqueous solution, enzymatic oxidizing-polymerizing reaction, separating to obtain tea red, tea yellow and tea brown, purifying, concentrating and drying.
Description
(1) technical field
The present invention relates to utilize the tea extract to produce the method for tea pigment, be specially the enzyme that utilizes tealeaves itself and add or do not add the enzyme bought from the market method of oxidized teas polyphenol generation tea pigment together.
(2) background technology
Tea pigment is the mixture of Polyphenols and derivative thereof in the tealeaves, and its major ingredient is theoflavin class, thearubigins class, theabrownin class.Wherein theoflavin class pharmacologically active is the strongest, at present in the world the demanding criteria of tea pigment mainly a kind of high-active tawny agent and production method thereof have been announced be as the criterion .2001 February 28 Chinese Patent Office of the content requirement of theoflavin, in please number be 00112536, be characterized in directly Fresh Folium Camelliae sinensis being smashed to pieces slagging and leaf, add buffered soln then, add or do not add the tea extract tea-polyphenol, under ventilation and suitable temperature condition, carry out the enzymatic oxidn polyreaction, generate tea pigment based on theoflavin, thearubigins.Utilize this method, though the tea pigment of production wherein the content of theoflavin can reach 50%, the yield of tea pigment has only 50%, the theoflavin yield is lower like this.The reason that the yield of theoflavin is low is that the oxidizing reaction of this method is to carry out in the aqueous solution, and growing amount and the temperature of reaction of theoflavin in water has substantial connection, temperature is lower, theoflavin is not soluble in water, the theoflavin that generates during reaction is attached to the surface of enzyme, during solid-liquid separation, theoflavin is discharged from solid enzyme slag; And in the higher aqueous solution of temperature, though theoflavin is soluble in water, deep oxidation generates thearubigins and theabrownin rapidly under enzymatic reaction, has influenced the yield of theoflavin.
(3) summary of the invention
At the shortcoming that yield is lower and technology is loaded down with trivial details of theoflavin in the method for above-mentioned production tea pigment, the invention provides another production method of tea pigment, the yield height of theoflavin, process optimization, production cost is low.
Its main technical schemes is: a kind of method of producing tea pigment is characterized in that:
A, the processing of enzyme:
With the bright leaf of tea pulverize, rub cut, micronizing, standby under-16 ℃～-18 ℃ conditions;
B, enzymatic reaction: tea-polyphenol is added wiring solution-forming in the organic solvent, add acidic aqueous solution then, add the enzyme of a processing again, temperature is controlled between 10 ℃～65 ℃, stirs the reaction 0.5～5 hour of ventilating; Wherein: the weight of tea-polyphenol: volume of organic solvent=1 kilogram: 5～50 liters; Volume of organic solvent: the volume of acidic aqueous solution=1～10: 1; The weight of enzyme: the weight of tea-polyphenol=1～10: 1;
C separates: will go out water, slag phase, organic phase through the solution separating that b handles;
D, purifying: with the isolating organic phase of purifying agent abstraction purification c, it extracts than being the volume of organic phase: the volume of purifying agent=1: 0.5～3, collect organic phase;
E concentrates: place the scraper plate thickener to concentrate the organic phase behind the d purifying, organic solvent is removed on the top, and it is 5～25% to carry out spraying drying that water is made into solid content, and 60～65 ℃ of the temperature of scraper plate thickener, vacuum tightness are 0.06Mpa～0.08Mpa; 190～230 ℃ of the inlet temperature of spray-drying tower, air outlet temperature are 80～110 ℃, feed rate 50～500L/h.
Also the organic phase behind the purifying can be placed the scraper plate thickener to be concentrated into paste, place vacuum drying oven to dry to powder then, drying temperature is 45～60 ℃, and vacuum tightness is 0.06～0.08Mpa.Described acidic aqueous solution is that the pH value is 5～6.5 aqueous solutions of organic acids, for example aqueous citric acid solution or acetic acid aqueous solution
In the processing of enzyme, pulverize at the bright leaf of tea, rub and cut, can add polysaccharide hydrolase after the micronizing.Described organic solvent is a kind of in ethyl acetate, Virahol, ethanol, the chloroform at least.
The present invention utilizes the enzyme of the stronger tealeaves of activity itself, do not add or add the enzyme of buying from the market, impel polyphenolic compound oxypolymerization to generate the tea pigment that is rich in theoflavin, the yield of tea pigment can reach 80%, wherein the content of theoflavin reaches as high as more than 60%, advantage of the present invention is that the process of polyphenolic compound oxypolymerization generation tea pigment is carried out in multi phase state, the characteristics of this multi phase state enzymatic reaction are: 1, the reaction system temperature influence weakens, theoflavin has good solubility in organic solvent at low temperatures, and under comparatively high temps, owing to be reflected in the organic phase and carry out, reaction temperature and easy to control has suppressed the polyreaction of theoflavin continuation to thearubigins and theabrownin.2, thearubigins and theabrownin are not soluble in organic solvent, and the thearubigins of aqueous phase and the enrichment of theabrownin have also suppressed theoflavin and continued oxidation.More than 2 yield and both obvious raisings of purity that impelled theoflavin.So just avoided oxidizing reaction of the prior art to carry out in the aqueous solution, growing amount and the temperature of reaction of theoflavin in water has substantial connection, lower, the higher shortcoming that all can have influence on the yield of theoflavin of temperature.
(4) description of drawings
Fig. 1 is a process flow sheet of the present invention.
(5) embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1: the Fresh Folium Camelliae sinensis 100Kg through precooling that aquatic foods are plucked smashs to pieces with stamp mill in the input reactor of back, add tea-polyphenol 100Kg, add then in the ethyl acetate solution of 500L, the acetic acid aqueous solution 500L that adds pH=6.5 again, the ventilation stirring reaction is after 300 minutes under 65 ℃ of conditions, be cooled to 15 ℃, be incubated 1 hour, isolate organic phase, additional proportion is 1: 0.5 a water, fully stirs 20 minutes, centrifugation then, obtain organic phase, delivering to temperature is 60 ℃, vacuum tightness is to be concentrated into paste in the scraper plate thickener of 0.06Mpa, and delivering to temperature then is 45 ℃, vacuum tightness is to dry to powder in the vacuum drying oven of 0.06Mpa.The yield of tea pigment is 70%, detects according to the Roberts method: theoflavin is 45%, and thearubigins is 4.5%, and theabrownin is 3.3%.
Embodiment 2: the Fresh Folium Camelliae sinensis 100Kg through precooling that aquatic foods are plucked smashs to pieces with stamp mill in the input reactor of back, add tea-polyphenol 10Kg, add then in the ethanolic soln of 500L, the aqueous citric acid solution 50L that adds pH=5 again, the ventilation stirring reaction is after 240 minutes under 40 ℃ of conditions, be cooled to 15 ℃, be incubated 1 hour, isolate organic phase, additional proportion is 1: 1 a water, fully stirs 20 minutes, centrifugation then, obtain organic phase, delivering to temperature is 62 ℃, be concentrated into paste in the scraper plate thickener of vacuum tightness 0.07pa, delivering to temperature then is 50 ℃, vacuum tightness is to dry to powder in the vacuum drying oven of 0.07Mpa.The yield of tea pigment is 70%, detects according to the Roberts method: theoflavin is 60%, and thearubigins is 4.5%, and theabrownin is 2.8%.
Embodiment 3: the Fresh Folium Camelliae sinensis 100Kg through precooling that aquatic foods are plucked smashs to pieces with stamp mill in the input reactor of back, add tea-polyphenol 33Kg, polysaccharide hydrolase 500g, add then in the aqueous isopropanol of 660L, the aqueous citric acid solution 220L that adds pH=6 again, the ventilation stirring reaction is after 180 minutes under 30 ℃ of conditions, be cooled to 15 ℃, be incubated 1 hour, isolate organic phase, 1: 2 water of additional proportion, fully stirred 20 minutes, be cooled to 15 ℃, be incubated 1 hour, centrifugation then, obtain organic phase, delivering to temperature is 63 ℃, vacuum tightness is to be concentrated into paste in the scraper plate thickener of 0.08Mpa, and delivering to temperature then is 55 ℃, vacuum tightness is to dry to powder in the vacuum drying oven of 0.08Mpa.The yield of tea pigment is 78%, detects according to the Roberts method: theoflavin is 35%, and thearubigins is 5.1%, and theabrownin is 3.1%.
Embodiment 4: the Fresh Folium Camelliae sinensis 100Kg through precooling that aquatic foods are plucked smashs to pieces with stamp mill in the input reactor of back, add tea-polyphenol 16Kg, polysaccharide hydrolase 500g, add then in the chloroformic solution of 480L, the aqueous citric acid solution 80L that adds pH=6.5 again, the ventilation stirring reaction is after 120 minutes under 20 ℃ of conditions, be cooled to 15 ℃, be incubated 1 hour, isolate organic phase, additional proportion is 1: 2.5 a water, fully stirred 20 minutes, be cooled to 15 ℃, be incubated 1 hour, centrifugation then, obtain organic phase, delivering to temperature is 64 ℃, vacuum tightness is to be concentrated into paste in the scraper plate thickener of 0.08Mp, adds deionized water and continues to concentrate and be deployed into solid content 25% after organic solvent is removed on the top, delivering to inlet temperature then is 190 ℃, the 50L spray tower spraying drying that air outlet temperature is 80 ℃ is to powder, and its feed rate is 500L/h.The yield of tea pigment is 68%, and the yield of tea pigment is 70% to detect according to the Roberts method: theoflavin is 42%, and thearubigins is 5%, and theabrownin is 3%.
Embodiment 5: with the Fresh Folium Camelliae sinensis 100Kg through precooling of aquatic foods harvesting, smashing the back to pieces with stamp mill drops in the reactor, add tea-polyphenol 12.5Kg, polysaccharide hydrolase 500g, add then in the ethyl acetate solution of 500L, the aqueous citric acid solution 62.5L that adds pH=5 again, the ventilation stirring reaction is after 30 minutes under 10 ℃ of conditions, isolate organic phase, additional proportion is 1: 3 a water, fully stirred 20 minutes, be cooled to 15 ℃, be incubated 1 hour, centrifugation then obtains organic phase, and delivering to temperature is 65 ℃, vacuum tightness is to be concentrated into paste in the scraper plate thickener of 0.06Mpa, adding deionized water continues to be deployed into solid content 5% after organic solvent is removed on concentrated top, solid content 5% is exactly the tea pigment that 5g is arranged in the solution of 100ml, and delivering to inlet temperature then is 230 ℃, the 50L spray tower spraying drying that air outlet temperature is 110 ℃ is to powder, and its feed rate is 50L/h.The yield of tea pigment is 80%, detects according to the Roberts method: theoflavin is 46%, and thearubigins is 4.8%, and theabrownin is 3.2%.
Claims (6)
1. method of producing tea pigment is characterized in that:
A, the processing of enzyme:
With the bright leaf of tea pulverize, rub cut, micronizing, standby under-16 ℃～-18 ℃ conditions;
B, enzymatic reaction: tea-polyphenol is added wiring solution-forming in the organic solvent, add acidic aqueous solution then, add the enzyme of a processing again, temperature is controlled between 10 ℃～65 ℃, stirs the reaction 0.5～5 hour of ventilating; Wherein: the weight of tea-polyphenol: volume of organic solvent=1 kilogram: 5～50 liters; Volume of organic solvent: the volume of acidic aqueous solution=1～10: 1; The weight of enzyme: the weight of tea-polyphenol=1～10: 1;
C separates: will go out water, slag phase, organic phase through the solution separating that b handles;
D, purifying: with the isolating organic phase of purifying agent abstraction purification c, it extracts than being the volume of organic phase: the volume of purifying agent=1: 0.5～3, collect organic phase;
E concentrates: place the scraper plate thickener to concentrate the organic phase behind the d purifying, organic solvent is removed on the top, and it is 5～25% to carry out spraying drying that water is made into solid content, and 60～65 ℃ of the temperature of scraper plate thickener, vacuum tightness are 0.06Mpa～0.08Mpa; 190～230 ℃ of the inlet temperature of spray-drying tower, air outlet temperature are 80～110 ℃, feed rate 50～500L/h.
2. a kind of method of producing tea pigment according to claim 1, it is characterized in that to place through the organic phase behind the d purifying scraper plate thickener to be concentrated into paste, place vacuum drying oven to dry to powder then, drying temperature is 45～60 ℃, and vacuum tightness is 0.06～0.08Mpa.
3. a kind of method of producing tea pigment according to claim 1, the pH value that it is characterized in that described acidic aqueous solution is 5～6.5.
4. a kind of method of producing tea pigment according to claim 1 is characterized in that described acidic aqueous solution is aqueous citric acid solution or acetic acid aqueous solution.
5. a kind of method of producing tea pigment according to claim 1 is characterized in that described organic solvent is a kind of in ethyl acetate, Virahol, ethanol, the chloroform at least.
6. a kind of method of producing tea pigment according to claim 1 is characterized in that in the processing of described enzyme, pulverizes at the bright leaf of tea, rubs and cut, can add polysaccharide hydrolase after the micronizing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101126564A CN1304586C (en) | 2003-12-13 | 2003-12-13 | Method for preparing tea pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101126564A CN1304586C (en) | 2003-12-13 | 2003-12-13 | Method for preparing tea pigment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1626668A true CN1626668A (en) | 2005-06-15 |
| CN1304586C CN1304586C (en) | 2007-03-14 |
Family
ID=34759851
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2003101126564A Expired - Fee Related CN1304586C (en) | 2003-12-13 | 2003-12-13 | Method for preparing tea pigment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1304586C (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696269B (en) * | 2009-10-29 | 2011-06-08 | 中国农业科学院茶叶研究所 | Method for preparing theabrownins by using tea polyphenols as raw materials |
| CN101691591B (en) * | 2009-09-30 | 2011-11-23 | 浙江派诺生物技术有限公司 | Industrial preparation method of 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 |
| CN101455257B (en) * | 2009-01-08 | 2012-02-22 | 云南农业大学 | Fermentation method for preparing theabrownin |
| CN102827896A (en) * | 2012-09-14 | 2012-12-19 | 向华 | Method for extracting theaflavin and theanine from tea leaves |
| CN103451233A (en) * | 2012-10-27 | 2013-12-18 | 陈小强 | Method for preparing theabrownin by taking tea polyphenol as active ingredients through adopting compound enzyme process |
| CN103652090A (en) * | 2013-12-18 | 2014-03-26 | 张松波 | Method for directly extracting theabrownin with pu'er tea serving as raw material |
| 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 |
| CN107372933A (en) * | 2017-07-06 | 2017-11-24 | 杭州丹娜生物科技有限公司 | A kind of preparation method of the compound theabrownin of feature |
| WO2022156615A1 (en) * | 2021-01-19 | 2022-07-28 | 江苏德和生物科技有限公司 | Preparation method for non-ester-type tea polyphenol rich in egc |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7076265B2 (en) * | 2003-09-26 | 2006-07-11 | Motorola, Inc. | Power reduction method for a mobile communication system |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031309C (en) * | 1992-12-29 | 1996-03-20 | 武汉市职工医学院 | Extraction method of tea pigment |
| CN1035660C (en) * | 1993-01-01 | 1997-08-20 | 江西省绿色工业(集团)公司 | Tea pigment and preparing process thereof |
| CN1328092A (en) * | 2000-06-08 | 2001-12-26 | 陈虎 | Process for extracting tea pigment and its application in treating hyperlipomia |
| CN1221178C (en) * | 2000-09-14 | 2005-10-05 | 赵剑 | High-active tawny agent and productive method thereof |
| CN1112110C (en) * | 2000-10-29 | 2003-06-25 | 刘志炯 | Process for extracting high-purity tea polyphenol, theapigment and theine |
-
2003
- 2003-12-13 CN CNB2003101126564A patent/CN1304586C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101455257B (en) * | 2009-01-08 | 2012-02-22 | 云南农业大学 | Fermentation method for preparing theabrownin |
| CN101691591B (en) * | 2009-09-30 | 2011-11-23 | 浙江派诺生物技术有限公司 | Industrial preparation method of theaflavin |
| CN101696269B (en) * | 2009-10-29 | 2011-06-08 | 中国农业科学院茶叶研究所 | Method for preparing theabrownins by using tea polyphenols as raw materials |
| 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 |
| CN102827896A (en) * | 2012-09-14 | 2012-12-19 | 向华 | Method for extracting theaflavin and theanine from tea leaves |
| CN103451233A (en) * | 2012-10-27 | 2013-12-18 | 陈小强 | Method for preparing theabrownin by taking tea polyphenol as active ingredients through adopting compound enzyme process |
| CN103451233B (en) * | 2012-10-27 | 2015-09-16 | 陈小强 | Be that raw material compound biological enzyme legal system is for theabrownin with tea-polyphenol |
| 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 |
| CN103652090A (en) * | 2013-12-18 | 2014-03-26 | 张松波 | Method for directly extracting theabrownin with pu'er tea serving as raw material |
| CN103652090B (en) * | 2013-12-18 | 2015-04-29 | 张松波 | Method for directly extracting theabrownin with pu'er tea serving as raw material |
| CN107372933A (en) * | 2017-07-06 | 2017-11-24 | 杭州丹娜生物科技有限公司 | A kind of preparation method of the compound theabrownin of feature |
| WO2022156615A1 (en) * | 2021-01-19 | 2022-07-28 | 江苏德和生物科技有限公司 | Preparation method for non-ester-type tea polyphenol rich in egc |
| US11911433B2 (en) | 2021-01-19 | 2024-02-27 | Jiangsu Dehe Biotechnology Co., Ltd. | Preparation method of non-ester tea polyphenols rich in EGC |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1304586C (en) | 2007-03-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1304586C (en) | Method for preparing tea pigment | |
| CN100593410C (en) | Method for preparing ganoderma spore oil | |
| US20220080333A1 (en) | Ultrasonic composite acidic water extraction method for cordyceps polysaccharide and cordycepin in cordyceps militaris | |
| CN101160327A (en) | Process for obtaining pectin | |
| CN102827896B (en) | Method for extracting theaflavin and theanine from tea leaves | |
| CN100453559C (en) | Method for separating lentinan | |
| CN102948607B (en) | Method for preparing rice bran protein through steam explosion-compound enzyme method | |
| CN108070039A (en) | A kind of method that polysaccharide and flavones are synchronously extracted from ampelopsis grossdentata | |
| US7595080B2 (en) | Method for preparing an extract of fruit of Sophora japonica containing isoflavone | |
| CN103073914B (en) | Method for extracting maize yellow pigment from maize protein | |
| CN111528315A (en) | Deep extraction process of matcha-derived bioactive ingredients | |
| CN101691591B (en) | Industrial preparation method of theaflavin | |
| CN102633764A (en) | Production process for preparing anthocyanin and pectin by black soya bean hull | |
| CN106754834A (en) | A kind of preparation technology of high activity papain | |
| CN101029320B (en) | Method for extracting bean mill cake isoflavone by cellulase synergistic supersonic wave | |
| CN104846031A (en) | Method for extracting oat beta-glucan through fermentation method | |
| CN108034682A (en) | The extraction process of sealwort entity small-molecular peptides | |
| CN105294881B (en) | Method for extracting peony pod crude polysaccharide from peony pods | |
| CN100370011C (en) | Method for extracting pumpkin seed oil and pumpkin seed protein | |
| CN102250980B (en) | Process for extracting theaflavin product | |
| CN1834106B (en) | Fermenting free hydralysis process for extracting saporin from yellow ginger | |
| CN102219652A (en) | Method for preparing water-soluble resveratrol from giant knotweed rhizome | |
| CN102277304B (en) | Aspergillus aculeatus bacterial strain and method for preparing 5,7,8,4'-tetrahydroxyisoflavone by using same | |
| CN101619098A (en) | Backward extraction method for extracting rapeseed protein by reverse micelle | |
| CN106083983A (en) | A kind of method preparing helexin from Fructus Sapindi Mukouossi |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070314 Termination date: 20181213 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |