CN103193832B - Method for extracting and separating high-purity tea polyphenol from tea leaves - Google Patents
Method for extracting and separating high-purity tea polyphenol from tea leaves Download PDFInfo
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- CN103193832B CN103193832B CN201310113218.3A CN201310113218A CN103193832B CN 103193832 B CN103193832 B CN 103193832B CN 201310113218 A CN201310113218 A CN 201310113218A CN 103193832 B CN103193832 B CN 103193832B
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Abstract
The invention relates to a method for extracting and separating high-purity tea polyphenol from tea leaves. The method comprises the steps that an adsorption solvent is prepared; crushed tea leaf pieces are extracted under the temperature of 65-75 DEG C; the extracting solution is distilled to recover the solvent, and adsorbs polar impurities by adding an adsorbent and then is filtered; the filtrate is distilled and concentrated; the concentrated solution is extracted by adding ethyl acetate; purified water with equal amount to the concentrated solution is added in the extract liquid and then the solvent is distilled, the remaining water phase is dried by spraying to obtain the high-purity tea polyphenol. The yield of the tea polyphenol prepared according to the method reaches up to 12 percent above, and the purity of the tea polyphenol is over 98 percent; and the method is practical and simple, the technological process is short, and the production efficiency is high.
Description
One, technical field
The present invention relates to a kind of method of extraction and isolation tea-polyphenol from tealeaves.Belong to biological extraction technology.
Two, technical background
Tea-polyphenol is tanned or tea tannin also known as tea, is the general name of Polyphenols of Tea, comprises flavanol compound, anthocyanin class, flavonoid, flavonols and phenolic acids etc.Wherein important with flavanol compound material.Tea-polyphenol is one of main component forming Tea color fragrance, is also one of main component having nourishing function in tealeaves.Wherein important with catechin, account for the 60%-80% of Polyphenols total amount; Catechin, primarily of the isoreactivity material tool removing toxic substances of several monomer composition such as EGC, DLC, EC, EGCG, GCG, ECG tea-polyphenol and radiation resistance, is described as " radiation jinx " by healthy and medical circle; Major function has the effect of Green Tea Extract; Anti-aging effects; Radiation resistance; The effect of anticancer; The effect etc. of antibiotic and sterilizing effect and inhibiting HIV.It is anticorrosion that tea-polyphenol can be used for food fresh keeping, has no side effect, edible safety.Tea-polyphenol infiltrates in other organism (mainly food), can extend storage period, prevents food from fading, and improves Mierocrystalline cellulose stability, the various nutritive ingredient of available protecting food.
At present, use the method for extraction and isolation high-purity tea polypenols aborning, mainly contain following three kinds of methods: 1 solvent-extraction process, 2 ion catch electron microscopy, 3 posts are separated preparation method.But the product purity obtained is not high, appearance luster is pale brown or blackish green, chemical composition residual and impurity is also many, and processing time is longer; Therefore improve the content of product and purity and enhance productivity and seem particularly important.
Three, summary of the invention
The object of this invention is to provide a kind of method of extraction and isolation tea-polyphenol from tealeaves, health rank is high, technique is simple, product purity is high tea-polyphenol production technique that it has; Theophylline and pigment is got rid of while adsorbing contaminant.
The inventive method is completed by following steps:
1, sorbent material is prepared;
2, tea raw material is crushed to 5-10 order by pulverizer;
3, the ethanol that the raw material after pulverizing adds 6 times of 80% content of raw material weight extracts 3 times continuously under the temperature condition of 75 DEG C, 3 hours each extraction times;
4, united extraction liquid, by extracting solution after merging under the condition of heating 65 DEG C, ethanol is reclaimed in vacuum distilling, after reclaiming ethanol completely, add deployed sorbent material and carry out adsorption precipitation, the add-on of sorbent material is 10% of concentrated solution volume, leaves standstill centrifuging separating and removing impurities after 12 hours;
5, the filtered liquid after impurity is removed, after the activated carbon powder adding raw material weight 2% stirs and adsorbs soluble impurity in 30 minutes at 60 DEG C of-75 DEG C of temperature, recentrifuge separating and filtering;
6, the filtered liquid after being separated, vacuum concentration to raw material weight 1: 1 time add concentrated solution 5 times amount ethyl acetate and extract, totally three times;
7, through acetic acid ethyl acetate extract, vacuum concentration, to the greatest extent dry, then add pure water that raw material weighs 1/2 and is again distilled to and reclaims ethyl acetate solvent completely, complete the conversion of liquid phase effective constituent simultaneously;
8, spraying dry or concentrate drying can obtain the pure white product of high purity color and luster.
The preparation of described sorbent material: sorbent material prescription is: sanitation-grade polymerize aluminum chloride 20%, chitosan 80%, add 4 times of pure water after above raw material is merged mixing to be stirred under the temperature condition of normal temperature and to dissolve completely, solution effective constituent concentration is now 20%, for subsequent use under being statically placed in normal temperature.
The present invention can accomplish that the disposable pure white tea-polyphenol productive rate of color and luster of producing is up to more than 12%, high purity about 98%, can save the production time shared by chromatography processes link that common process produces product employing in a large number.
Four, embodiment
Embodiment 1:
(1), sorbent material is prepared: sorbent material prescription is: sanitation-grade polymerize aluminum chloride 20%, chitosan 80%, add 4 times of pure water after above raw material is merged mixing to be stirred under the temperature condition of normal temperature and to dissolve completely, solution effective constituent concentration is now 20%, for subsequent use under being statically placed in normal temperature.
(2) tea raw material 100 grams of pulverizing, is taken;
(3), the ethanol 600 milliliters of 6 times of concentration 80% of raw material weight, continuous circumfluence extraction 3 times under the temperature condition of 75 DEG C, 3 hours each extraction times is added;
(4) ethanol in extracting solution is reclaimed in the extracting solution vacuum distilling under 75 DEG C of temperature condition, merging 3 times, add deployed adsorbent solution 100 milliliters and carry out impurity absorption after ethanol reclaims, leave standstill centrifugation after 24 hours and filter and remove solid impurity;
(5), vacuum concentration filtered liquid after treatment again, reach the mass ratio 2: 1 of raw material and concentrated solution, both the raw material of 100 grams: the concentrated solution of 50 milliliters;
(6), the ethyl acetate that adds 6 times of volumes (300 milliliters) in concentrated solution extracts, totally 3 times;
(7), extraction liquid vacuum distilling at the temperature of 60 DEG C of combined ethyl acetate, first in extraction liquid, adds the pure water identical with concentrated solution volume before heating, while completing solvent recuperation, completes the conversion of effective constituent in two liquid solution;
(8) aqueous solution spraying dry, after solvent distillation.Weigh gained 127 grams after dry, the product that colourity is whiter, content reaches 98.2% after testing.
Embodiment 2:
(1), sorbent material is prepared: sorbent material prescription is: sanitation-grade polymerize aluminum chloride 20%, chitosan 80%, add 4 times of pure water after above raw material is merged mixing to be stirred under the temperature condition of normal temperature and to dissolve completely, solution effective constituent concentration is now 20%, for subsequent use under being statically placed in normal temperature;
(2) tea raw material of pulverizing, is taken: 100 kilograms;
(3), the ethanol 600 kilograms of 6 times of concentration 80% of raw material weight, continuous circumfluence extraction 3 times under the temperature condition of 75 DEG C, 3 hours each extraction times is added;
(4) ethanol in extracting solution is reclaimed in the extracting solution vacuum distilling under 75 DEG C of temperature condition, merging 3 times, add deployed adsorbent solution 100 kilograms and carry out impurity absorption after ethanol reclaims, leave standstill centrifugation after 24 hours and filter and remove solid impurity;
(5), vacuum concentration filtered liquid after treatment again, reach the mass ratio 2: 1 of raw material and concentrated solution, both the raw material of 100 kilograms: the concentrated solution of 50 kilograms;
(6), the ethyl acetate that adds 6 times of volumes (300 kilograms) in concentrated solution extracts, totally 3 times.
(7), extraction liquid vacuum distilling at the temperature of 60 DEG C of combined ethyl acetate, first in extraction liquid, adds the pure water identical with concentrated solution volume before heating, while completing solvent recuperation, completes the conversion of effective constituent in two liquid solution;
(8) aqueous solution spraying dry, after solvent distillation.Weigh gained 12.8 kilograms after dry, the product that colourity is whiter, content reaches 98.37% after testing.
Embodiment 3:
(1), sorbent material is prepared: sorbent material prescription is: sanitation-grade polymerize aluminum chloride 20%, chitosan 80%, add 4 times of pure water after above raw material is merged mixing to be stirred under the temperature condition of normal temperature and to dissolve completely, solution effective constituent concentration is now 20%, for subsequent use under being statically placed in normal temperature;
(2) tea raw material of pulverizing, is taken: 200 kilograms;
(3), the ethanol 1200 kilograms of 6 times of concentration 80% of raw material weight, continuous circumfluence extraction 3 times under the temperature condition of 75C, 3 hours each extraction times is added;
(4) ethanol in extracting solution is reclaimed in the extracting solution vacuum distilling under 75 DEG C of temperature condition, merging 3 times, add deployed adsorbent solution 200 kilograms and carry out impurity absorption after ethanol reclaims, leave standstill centrifugation after 24 hours and filter and remove solid impurity;
(5), vacuum concentration filtered liquid after treatment again, reach the mass ratio 2: 1 of raw material and concentrated solution, both the raw material of 200 kilograms: the concentrated solution of 100 kilograms;
(6), the ethyl acetate that adds 6 times of volumes (600 kilograms) in concentrated solution extracts, totally 3 times;
(7), extraction liquid vacuum distilling at the temperature of 60 DEG C of combined ethyl acetate, first in extraction liquid, adds the pure water identical with concentrated solution volume before heating, while completing solvent recuperation, completes the conversion of effective constituent in two liquid solution;
(8) aqueous solution spraying dry, after solvent distillation.Weigh gained 25.7 kilograms after dry, the product that colourity is whiter, content reaches 98.31% after testing.
Claims (2)
1. the method for extraction and isolation tea-polyphenol from tealeaves, is characterized in that: the inventive method is completed by following steps:
(1), sorbent material is prepared;
(2), tea raw material is crushed to 5-10 order by pulverizer;
(3), pulverize after the raw material ethanol that adds 6 times of 80% content of raw material weight extract 3 times continuously under the temperature condition of 75 DEG C, 3 hours each extraction times;
(4), united extraction liquid, by extracting solution after merging under the condition of heating 65 DEG C, ethanol is reclaimed in vacuum distilling, after reclaiming ethanol completely, add deployed sorbent material and carry out adsorption precipitation, the add-on of sorbent material is 10% of concentrated solution volume, leaves standstill centrifuging separating and removing impurities after 12 hours;
(5), the filtered liquid after impurity is removed, after the activated carbon powder adding raw material weight 2% stirs and adsorbs soluble impurity in 30 minutes at 60 DEG C of-75 DEG C of temperature, recentrifuge separating and filtering;
(6), be separated after filtered liquid, vacuum concentration to raw material weight 1: 1 time add concentrated solution 5 times amount ethyl acetate and extract, totally three times;
(7), through acetic acid ethyl acetate extract, vacuum concentration, to the greatest extent dry, then add pure water that raw material weighs 1/2 and is again distilled to and reclaims ethyl acetate solvent completely, complete the conversion of liquid phase effective constituent simultaneously;
(8), spraying dry or concentrate drying can obtain the pure white product of high purity color and luster.
2. the method for a kind of extraction and isolation high-purity tea polypenols from tealeaves as claimed in claim 1, it is characterized in that the preparation of sorbent material, sorbent material prescription is: sanitation-grade polymerize aluminum chloride 20%, chitosan 80%, add 4 times of pure water after above raw material is merged mixing to be stirred under the temperature condition of normal temperature and to dissolve completely, solution effective constituent concentration is now 20%, for subsequent use under being statically placed in normal temperature.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105885851A (en) * | 2014-11-14 | 2016-08-24 | 上海霖成生物科技有限公司 | Pineapple peel extract and preparation method thereof |
| CN107455521A (en) * | 2017-08-16 | 2017-12-12 | 广西克鲁尼茶叶生物科技有限公司 | A kind of complex art for being used for the high efficiency extraction Tea Polyphenols from discarded tealeaves |
| CN111850567A (en) * | 2020-07-10 | 2020-10-30 | 南京航空航天大学 | Non-toxic corrosion inhibitor and preparation method thereof |
| CN111838666A (en) * | 2020-08-10 | 2020-10-30 | 桑迪(武汉)生物科技有限公司 | Composition with auxiliary memory improving function and application thereof |
| CN113598370A (en) * | 2021-08-06 | 2021-11-05 | 厦门稀土材料研究所 | Effective part extract of tea waste and extraction method and application thereof |
| CN114042114A (en) * | 2021-11-17 | 2022-02-15 | 宜兴市天石饲料有限公司 | Preparation method of tea polyphenol by adopting ethyl acetate extraction |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08109178A (en) * | 1994-10-11 | 1996-04-30 | Mitsui Norin Kk | Production of low-caffeine tea polyphenol |
| CN1161321A (en) * | 1996-09-28 | 1997-10-08 | 浙江大学 | Method for extracting tea polyphenol and by-products from tea leaves |
| CN1709887A (en) * | 2005-07-13 | 2005-12-21 | 东北林业大学 | Method for preparing high-purity tea polypenols |
| CN101643483A (en) * | 2009-05-26 | 2010-02-10 | 苏州派腾生物医药科技有限公司 | Process for preparing tea polyphenol |
| CN102432091A (en) * | 2011-10-27 | 2012-05-02 | 常州大学 | Preparation method of composite flocculating agent for pretreating blue alga biogas slurry |
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- 2013-03-30 CN CN201310113218.3A patent/CN103193832B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08109178A (en) * | 1994-10-11 | 1996-04-30 | Mitsui Norin Kk | Production of low-caffeine tea polyphenol |
| CN1161321A (en) * | 1996-09-28 | 1997-10-08 | 浙江大学 | Method for extracting tea polyphenol and by-products from tea leaves |
| CN1709887A (en) * | 2005-07-13 | 2005-12-21 | 东北林业大学 | Method for preparing high-purity tea polypenols |
| CN101643483A (en) * | 2009-05-26 | 2010-02-10 | 苏州派腾生物医药科技有限公司 | Process for preparing tea polyphenol |
| CN102432091A (en) * | 2011-10-27 | 2012-05-02 | 常州大学 | Preparation method of composite flocculating agent for pretreating blue alga biogas slurry |
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Effective date of registration: 20151027 Address after: 723500, a group of villages in Chengguan Town, Chengguan County, Hanzhoung City, Shaanxi Province, Xixiang Patentee after: Shaanxi Qin natural biological science and Technology Co Ltd Address before: 712000 Xianyang province Shaanxi City Weicheng district emerging North Bureau 14 iron building No. 101 Patentee before: Wang Xijun |
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Effective date of registration: 20181206 Address after: 710018 Unit 1603, No. 6, No. 2, Kunming Road, Lianhu District, Xi'an City, Shaanxi Province Patentee after: Xi'an Zhengdong Biotechnology Co., Ltd. Address before: 712000 No. 101, Building 14, Xinyun Branch, Xinxing North Railway Bureau, Weicheng District, Xianyang City, Shaanxi Province Patentee before: Wang Xijun |
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