CN1351012A - Process for extracting high-purity tea polyphenol, theapigment and theine - Google Patents

Process for extracting high-purity tea polyphenol, theapigment and theine Download PDF

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Publication number
CN1351012A
CN1351012A CN 00120528 CN00120528A CN1351012A CN 1351012 A CN1351012 A CN 1351012A CN 00120528 CN00120528 CN 00120528 CN 00120528 A CN00120528 A CN 00120528A CN 1351012 A CN1351012 A CN 1351012A
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tea
water
polyphenol
weight
obtains
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CN1112110C (en
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刘志炯
卢东
全力
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Shanxi East Horse Biological Medicine Polytron Technologies Inc
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  • Coloring Foods And Improving Nutritive Qualities (AREA)
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Abstract

A process for extracting high-purity tea polyphenol, theapigment and theine from tea leaves includes such steps as immersing broken tea leaves in warm water, microfilter to prepare extract liquid, adding complex salt (zinc sulfate-calcium chloride) for deposition, separating deposit from filtrate, washing deposit in water, dissolving in sulfuric acid, recovering ethyl acetate by organic phase to prepare extract, dissolving in water, extracting in ether, recovering ether by organic phase, drying to obtain tea polyphenol, recovering ether by water phase, drying to obtain theoflavin, mixing filtrate with water-washing liquid, extracting by dichloromethane, and recovering dichloromethane to obtain theine and tea red pigment. Its advantages are high purity and low cost.

Description

Extract high-purity tea polypenols tea pigment tea trimethyl-xanthine technology from tealeaves
The invention belongs to and from tealeaves, extract tea-polyphenol, tea pigment, tea trimethyl-xanthine Technology field.
Contain compositions such as tea-polyphenol, tea pigment, tea trimethyl-xanthine element in the tealeaves extract, wherein tea-polyphenol have anti-oxidant, prolong aging, suppress cancer, effects such as treatment cardiovascular and cerebrovascular disease; That tea pigment has is anti-oxidant, the effect of mutation inhibiting, anti-ageing, the multiple geriatric disease of treatment; The tea trimethyl-xanthine has and efficiently enlivens cell, anticancer effect.Prior art, for example Chinese patent application 88108154.X " a kind of method of extracting natural antioxidants from tealeaves ", 91109901.8 " extracting method of tea natural antioxidant one tea-polyphenol ", 93110906.X " tea polyphenols serial health drink ", 88108725.4 " producing the processing method of caffeine from the tealeaves tankage ", 91103543.5 " production methods of green tea caffeine " disclose the processing method of extracting tea-polyphenol or tea pigment or tea trimethyl-xanthine from tealeaves.Above prior art, have be a kind of from tealeaves the processing method of one of extracting effective components, remaining effective constituent then got rid of thrown aside, extraction and application in addition is very not unfortunate; Though what have can extract tea-polyphenol, tea pigment and tea trimethyl-xanthine, its purity and recovery rate are all not high; Boiling water soaks for a long time, the highly basic precipitation and the preparation immersion liquid is all adopted, and for example the high pH value precipitation of calcium hydroxide makes the tea-polyphenol oxidation, causes purity and recovery rate not high.
The object of the present invention is to provide a kind of employing room temperature water to soak tea dust, membrane technique removal of impurities, double salt precipitation, aqueous phase organic solvent recovery and utilization technology from tealeaves extraction high-purity tea polypenols tea pigment tea trimethyl-xanthine technology.
The object of the present invention is achieved like this: a kind of from tealeaves extraction high-purity tea polypenols tea pigment tea trimethyl-xanthine technology, its technology is as follows:
A, preparation immersion liquid: with the polygalacturonase of 20-40 order tea dust and its weight 0.01-0.03%, be soaked in 5-7 times of room temperature water of tea dust weight about 24 hours, dash with steam and carry 10-20 minute; Carry out micro-filtration with 0.5 μ m micropore fine filtration device; With the heavy 0.5-1 of tea dust hot water injection doubly; Carry out ultrafiltration with 40000-50000 dalton fenestra ultra-fine filter, remove pectin, protein impurities, the immersion liquid of being infused clearly.
B, double salt precipitation separate: in the immersion liquid that a obtains, add its weight 5-7% ratio and be (3-4): 1 zinc sulfate and calcium chloride double salt are adjusted to about 6 with the 0.5-0.7M sodium hydrogen carbonate solution with its pH value and make it precipitation fully; Carry out micro-filtration, the precipitation that will contain the tea-polyphenol theoflavin is separated with the filtrate that contains tea trimethyl-xanthine tea red pigment.
C, preparation medicinal extract: the tea-polyphenol theoflavin precipitation that contains that b obtains is washed with water; Precipitation after the washing is with the 3-5M sulfuric acid dissolution; Carrying out micro-filtration removes slag; The extraction of weight ethyl acetates such as acid solution adding, its organic phase reclaims ethyl acetate, obtains containing tea-polyphenol theoflavin medicinal extract; The ethyl acetate that reclaims is returned in the acid solution of this operation.
D, preparation high-purity tea polypenols and theoflavin: contain tea-polyphenol theoflavin medicinal extract with its 5-7 times of weight water dissolution with what c obtained, weight extracted with diethyl ether such as adding, its organic phase reclaims ether, with the gained solid drying, obtains high-purity tea polypenols;
After its water reclaims ether, add and wait the weight ethyl acetate extraction, the recovery ethyl acetate with the gained solid drying, obtains high-purity theaflavin;
E, preparation tea trimethyl-xanthine and tea red pigment: contain tea trimethyl-xanthine tea red pigment filtrate with what b obtained, mix with water lotion among the c; Add and to be about half dichloromethane extraction of mixed solution weight;
Organic phase reclaims methylene dichloride, obtains tea trimethyl-xanthine crude product, refining finished product; Water reclaims the methylene dichloride after drying, obtains tea red pigment.
With C obtain contain tea-polyphenol and theoflavin medicinal extract carries out drying, can obtain coarse-grain attitude tea-polyphenol.
Advantage of the present invention is to utilize the tealeaves tankage comprehensively to extract tea-polyphenol, tea pigment and tea trimethyl-xanthine, makes full use of starting material and save energy, increases recovery rate, reduces cost; Do not use boiling water to soak in the technology, avoid oxidation, increase recovery rate effective constituent; Comprehensive membrane technique removal of impurities and the double salt precipitation of using improves the quality of products; The organic solvent that uses in the technology gives recycling use, has reduced cost, reduces environmental pollution; The quality product height, tea-polyphenol purity can reach 99.5%, and contained tea pigment can reach 95% in the theoflavin, and contained tea pigment can reach 60% in the tea red pigment, and tea trimethyl-xanthine quality reaches 23 editions quality standards of American Pharmacopeia.
Fig. 1 is a process flow diagram of the present invention.Fig. 1 is described as follows: 1 is the preparation immersion liquid, and 2 for double salt precipitation separates, and 3 are preparation medicinal extract, and 4 are preparation high-purity tea polypenols and theoflavin, and 5 are preparation tea trimethyl-xanthine and tea red pigment.
One embodiment of the present of invention are as follows:
A, 200 kilograms of 20-40 order tealeaves tankage are added 0.02 kilogram of 1000 kilograms of room temperature waters and polygalacturonase, soaked 24 hours; Dash with steam and to carry 15 minutes; Carry out micro-filtration with 0.5 μ m accurate filter; Pump into 70 ℃ of hot water and in filter, wash, discard dregs; Carry out ultrafiltration with 50000 dalton's fenestra ultra-fine filters, remove the immersion liquid that impurity is infused clearly.
Add 3 kilograms in 9 kilograms in zinc sulfate and calcium chloride in b, the immersion liquid, transferring pH value with the sodium hydrogen carbonate solution of 0.6M is 6, makes tea-polyphenol and theoflavin precipitation fully, carries out micro-filtration;
C, the throw out washing that b is obtained; Precipitation after washing is carried out micro-filtration with the 3.5M sulfuric acid dissolution, discards dregs; Acid solution with etc. the ethyl acetate extraction of weight, organic phase reclaim under reduced pressure ethyl acetate, tea-polyphenol medicinal extract, the ethyl acetate of recovery is returned in the acid solution of this operation.
D, the medicinal extract that c is obtained, with 6 times of water dissolution, the extracted with diethyl ether of weight such as adding, its organic phase reclaims ether, resulting solid after lyophilize, purity reach 99.5% tea-polyphenol;
After its water reclaims ether, the ethyl acetate extraction of weight such as adding, the reclaim under reduced pressure ethyl acetate, the solid of gained gets purity and reaches 95% theoflavin through lyophilize.
E, filtrate that b is obtained mix with water lotion among the c, add the dichloromethane extraction of half amount, and methylene dichloride is reclaimed in its organic phase distillation, obtains the tea trimethyl-xanthine; Its water obtains tea red pigment through the thin film evaporation drying after reclaiming methylene dichloride.

Claims (2)

1, a kind of from tealeaves extraction high-purity tea polypenols tea pigment tea trimethyl-xanthine technology, it is characterized in that technology is as follows:
A, preparation immersion liquid:, be soaked in the tea dust weight 5-7 room temperature water doubly about 24 hours with the polygalacturonase of 20-40 order tea dust and its weight 0.01-0.03%; Dash with steam and to carry 10-20 minute; Carry out micro-filtration with 0.5 μ m accurate filter; With the heavy 0.5-1 times of hot water injection of tea dust; Carry out ultrafiltration with 40000-50000 dalton fenestra ultra-fine filter, remove pectin, protein impurities, the immersion liquid of being infused clearly;
B, double salt precipitation separate: in the immersion liquid that a obtains, add its weight 5-7% ratio and be (3-4): 1 zinc sulfate and calcium chloride double salt; With the 0.5-0.7M sodium hydrogen carbonate solution its pH value is adjusted to about 6, makes it precipitation fully; Carry out micro-filtration, the precipitation that will contain the tea-polyphenol theoflavin is separated with the filtrate that contains tea trimethyl-xanthine tea red pigment;
C, preparation medicinal extract: the tea-polyphenol theoflavin precipitation that contains that b obtains is washed with water; Precipitation after the washing is with the 3-5M sulfuric acid dissolution; Carrying out micro-filtration removes slag; The ethyl acetate extraction of weight such as acid solution adding, its organic phase reclaims ethyl acetate, obtains containing tea-polyphenol theoflavin medicinal extract; The ethyl acetate that reclaims is returned in the acid solution of this operation;
D, preparation high-purity tea polypenols and theoflavin: contain tea-polyphenol theoflavin medicinal extract with its 5-7 times of weight water dissolution with what c obtained; The extracted with diethyl ether of weight such as adding, its organic phase reclaims ether, with the gained solid drying, obtains high-purity tea polypenols;
After its water reclaimed ether, the ethyl acetate extraction of weight such as adding reclaimed ethyl acetate, with the gained solid drying, got high-purity theaflavin;
E, preparation tea trimethyl-xanthine and tea red pigment; The tea trimethyl-xanthine tea red pigment filtrate that contains that b obtains is mixed with water lotion among the c; Add and to be about half dichloromethane extraction of mixed solution weight;
Organic phase reclaims methylene dichloride, obtains tea trimethyl-xanthine crude product refining and gets finished product; Water reclaims the methylene dichloride after drying, obtains tea red pigment.
2, described a kind of according to claim 1 from tealeaves extraction high-purity tea polypenols tea pigment tea trimethyl-xanthine technology, it is characterized in that the tea-polyphenol theoflavin medicinal extract that c is obtained carries out drying, obtains coarse-grain attitude tea-polyphenol.
CN 00120528 2000-10-29 2000-10-29 Process for extracting high-purity tea polyphenol, theapigment and theine Expired - Fee Related CN1112110C (en)

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN1317966C (en) * 2004-07-19 2007-05-30 陈忠 Tea essence for tea food and its preparation method
CN100374027C (en) * 2004-03-24 2008-03-12 上海市农业科学院作物育种栽培研究所 Extraction process of plant mildew-proof preservative
CN101142957B (en) * 2007-10-09 2010-09-15 浙江大学 Method for extracting green tea concentrated liquid
CN101575326B (en) * 2009-06-25 2011-05-04 合肥工业大学 Method for extracting tea polyphenol from glede tea
CN101508690B (en) * 2009-03-17 2011-05-11 林峰 Novel methods for simultaneously extracting tea polyphenol, tea polysaccharide and caffeinum from tea
CN103012403A (en) * 2013-01-05 2013-04-03 四川中测科技投资有限公司 Tea leaf comprehensive utilizing and deep processing method
CN104306559A (en) * 2014-10-14 2015-01-28 王惠莹 Preparation method of golden camellia leaf pigment
CN104846029A (en) * 2015-04-22 2015-08-19 湖南农业大学 Preparation method of simple theaflavin monomer
CN106070840A (en) * 2016-06-16 2016-11-09 浙江大学 Preparation has the method for the water alcohol compatibility Folium Camelliae sinensis extract of tea scented tea color
CN106728417A (en) * 2017-01-18 2017-05-31 俞镜含 A kind of gentle method for extracting Tea Pigment
CN111035696A (en) * 2019-12-16 2020-04-21 格律药业有限公司 Pharmaceutical composition containing tea extract and its use for treating cancer
CN111035697A (en) * 2019-12-31 2020-04-21 格律药业有限公司 Pharmaceutical composition and application thereof, preparation method of nanoparticles, extraction process of tea extract and tea extract

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN100374027C (en) * 2004-03-24 2008-03-12 上海市农业科学院作物育种栽培研究所 Extraction process of plant mildew-proof preservative
CN1317966C (en) * 2004-07-19 2007-05-30 陈忠 Tea essence for tea food and its preparation method
CN101142957B (en) * 2007-10-09 2010-09-15 浙江大学 Method for extracting green tea concentrated liquid
CN101508690B (en) * 2009-03-17 2011-05-11 林峰 Novel methods for simultaneously extracting tea polyphenol, tea polysaccharide and caffeinum from tea
CN101575326B (en) * 2009-06-25 2011-05-04 合肥工业大学 Method for extracting tea polyphenol from glede tea
CN103012403A (en) * 2013-01-05 2013-04-03 四川中测科技投资有限公司 Tea leaf comprehensive utilizing and deep processing method
CN103012403B (en) * 2013-01-05 2015-03-11 四川中测科技投资有限公司 Tea leaf comprehensive utilizing and deep processing method
CN104306559A (en) * 2014-10-14 2015-01-28 王惠莹 Preparation method of golden camellia leaf pigment
CN104846029A (en) * 2015-04-22 2015-08-19 湖南农业大学 Preparation method of simple theaflavin monomer
CN104846029B (en) * 2015-04-22 2017-12-29 湖南农业大学 A kind of preparation method of simple kinds of theaflavin monomer
CN106070840A (en) * 2016-06-16 2016-11-09 浙江大学 Preparation has the method for the water alcohol compatibility Folium Camelliae sinensis extract of tea scented tea color
CN106728417A (en) * 2017-01-18 2017-05-31 俞镜含 A kind of gentle method for extracting Tea Pigment
CN111035696A (en) * 2019-12-16 2020-04-21 格律药业有限公司 Pharmaceutical composition containing tea extract and its use for treating cancer
CN111035697A (en) * 2019-12-31 2020-04-21 格律药业有限公司 Pharmaceutical composition and application thereof, preparation method of nanoparticles, extraction process of tea extract and tea extract

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