CN1699586A - Process for extracting tea polyphenol, caffeine as a byproduct thereof and tea polysaccharide from tea - Google Patents
Process for extracting tea polyphenol, caffeine as a byproduct thereof and tea polysaccharide from tea Download PDFInfo
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- CN1699586A CN1699586A CN 200510042629 CN200510042629A CN1699586A CN 1699586 A CN1699586 A CN 1699586A CN 200510042629 CN200510042629 CN 200510042629 CN 200510042629 A CN200510042629 A CN 200510042629A CN 1699586 A CN1699586 A CN 1699586A
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Abstract
Disclosed is a process for extracting tea polyphenol, caffeine as a byproduct thereof and tea polysaccharide from tea, which comprises, (1) extracting active ingredients including tea polyphenol, caffeine and tea polysaccharide from the tea through composite enzymolysis abstraction and water abstraction, (2) filtering the raffinate with hyperfiltration membrane, (3) subjecting the membrane compression liquid to ethanol deposition so as to obtain crude polysaccharides, removing protein and carrying out ethanol deposition, drying to obtain the tea polysaccharides, (4) separating and purifying through second level resin adsorption chromatography, thus obtaining tea polyphenol as well as caffeine as by-product.
Description
Technical field
The present invention relates to a kind of processing method of from tealeaves, extracting tea-polyphenol by-product trimethyl-xanthine and tea polysaccharide.
Background technology
Tea-polyphenol is pure natural, multi-functional, dynamical excellent anti oxygenant and radical scavenger.The nourishing function of tea-polyphenol mainly contains eliminates interior free yl, anti-ageing and anticancer, radioprotective and antibiotic, sterilization etc., and it is fresh-keeping to be widely used in the varieties of food items antioxygen, and fields such as Medicines and Health Product, makeup, household chemicals.Trimethyl-xanthine has the stimulating central nervous system system, human body is had physiology and health-care effects such as cardiac stimulant, diuresis, detoxifcation, is the important source material of medicine, healthcare products, beverage etc.That tea polysaccharide has is hypoglycemic, reducing blood-fat, anticoagulation, antithrombotic, hypoxia tolerance and enhancing body immunizing power, anti-inflammatory, multiple pharmacological effect such as anticancer, is expected to become the natural drug of prevention and treatment diabetes and cardiovascular disorder, raise immunity.
The production of tea-polyphenol mainly contains solvent extration, ion precipitation method, supercritical extraction, resin adsorption method etc. at present.Before several method have that solvent consumption is big, yield is low, energy consumption is high, have poisonous dissolvent residual, problem such as process complexity, facility investment are big.Resin adsorption method has that technology is simple, energy consumption is lower, safely, help realizing characteristics such as scale operation.But general resin absorption technique, existence does not cause product purity low because of Choice of Resin is high, particularly caffeine content exceeds standard, thereby must not be no longer with traditional technology caffein-frees such as solvent extractions, perhaps the Choice of Resin height but makes ethanolic soln problem such as wash-out fully too by force because of the adsorptive power to tea-polyphenol.
● Chinese patent application (200410015905.2) has reported that a kind of microwave-assisted extracts, salt precipitation tea polysaccharide, chloroform extraction trimethyl-xanthine, the production method of ethyl acetate extraction tea-polyphenol.Though this technology can be produced multiple product, but the production technique of tea-polyphenol, trimethyl-xanthine is not still broken away from chloroform and the solvent-extracted traditional old road of ethyl acetate, it is poor also to have production security, there is harmful dissolvent residual in the product, influence its problem such as application at field of food, the yield of tea-polyphenol and purity are also all lower.
● Chinese patent application (application number 02135864.8) has been reported a kind of improved ion precipitation method: change molten, ethyl acetate extraction tea-polyphenol with boiling water extraction, ion precipitation, hydrochloric acid, these and traditional ion precipitation method and indistinction.Increased in this patent the freezing of extraction liquid left standstill removal of impurities, though the refrigerating process that helps improving the quality of products has improved energy consumption and production cost greatly.
● Xibei College of Light Industry's journal, 2002,20 (5): 1-8, " adsorption resin method prepares the technical study of tea-polyphenol elaboration " of report is extraction solvent with 80% ethanol, with NKA-2 macroporous adsorbent resin separating tea multi-phenol.Because this resin choice is not high enough, in order to improve product purity, has added the ethyl acetate extraction step after the absorption twice.As seen this technology drawback that still can not avoid solvent extraction and bring, this is the existing common issue with of present resin method.
● spectroscopy and spectroscopic analysis, 2003,23 (1): 143-145, " polyamide resin is to the tea-polyphenol and the research of caffeine adsorption selectivity " of report has studied the adsorption separation performance of polyamide resin to tea-polyphenol and caffeine.Though polyamide resin is better to the adsorption selectivity of tea-polyphenol, but because so it is lower with the alcoholic acid eluting rate by force with the hydrogen bond action of tea-polyphenol, polyamide resin is unformed state in addition, and therefore not withstand voltage, easy pollution very is not fit to large-scale industrial production.
● Japanese Patent (JP8109178) has been reported the method with hot water, organic solvent extraction, and extracting solution uses the technology of synthetic adsorbent adsorbing and removing trimethyl-xanthine under alkaline condition (pH7-14), but very easily oxidational losses of tea-polyphenol under the alkaline condition.
● Chinese patent (96113134.9) has been reported a kind of method of extracting tea-polyphenol and byproduct thereof in tealeaves, with aqueous ethanol lixiviate tealeaves, adds the translucent precipitation of acid generation in the extracting solution and gets tea polysaccharide through the ultrafiltration after drying; Ultrafiltrated generates the tea-polyphenol precipitation through calcium chloride and alkali, and ion exchange resin column is crossed in the molten back of acid, again through aqueous ethanol wash-out, distillation concentrate, spraying drying gets the tea-polyphenol product.This technology has added the ion-exchange purification process on the basis of the conventional ion precipitator method, technology is numerous and diverse, in addition, and the recovery process energy consumption height of trimethyl-xanthine.
● Zhang, X. etc. (chemical engineering, 2001,29 (3): 15-19 has reported with hot water extraction, extracting solution is used the polyamide resin Adsorption of Tea Polyphenols after cellulose acetate composite titanium super-filter micro-porous membrane is refining, the liquid that sees through of polyamide resin column uses the XDA resin absorption to reclaim the technology of trimethyl-xanthine again.The adsorption selectivity of polymeric amide is better, but eluting rate is unsatisfactory, only is 50%-60% as the static desorption rate of 85% alcoholic acid.
● research and development of natural products .1999,11 (6): 44-49, report " use the resin fractionation by adsorption and produce tea-polyphenol " introduced boiling water extraction, the NKA-9 macroporous resin adsorption, methylene dichloride wash-out trimethyl-xanthine, the ethanol elution tea-polyphenol is produced the method for tea-polyphenol raw product.At present, the macroporous resin of the overwhelming majority can elute tea-polyphenol and trimethyl-xanthine simultaneously with ethanol, does not have the wash-out centrifugation.Therefore, it adopts methylene dichloride wash-out trimethyl-xanthine, and this has brought problems such as noxious solvent is residual equally.In addition, methylene dichloride brings problem also can for secular industrial applications to the swelling of resin.
Summary of the invention
At the shortcoming that exists in the present tea-polyphenol production technique, the purpose of this invention is to provide a kind of method of from tealeaves, extracting tea-polyphenol and by-product trimethyl-xanthine and tea polysaccharide efficiently, utilize the high characteristics of enzymolysis and extraction tea polysaccharide extraction yield, by ultrafiltration the refining of extracting solution and recovery tea polysaccharide are organically combined, the utilization ratio and the productivity effect of tealeaves have been improved, avoided simultaneously using deleterious organic solvent wash-out or extraction process caffein-free process, with tea-polyphenol and trimethyl-xanthine high efficiency separation.
A kind of processing method of from tealeaves, extracting tea-polyphenol by-product trimethyl-xanthine and tea polysaccharide, its steps in sequence is as follows:
(A) effective constituents such as tea-polyphenol, trimethyl-xanthine and tea polysaccharide in extraction of employing complex enzyme hydrolysis and the water extraction tealeaves;
(B) extracting solution is through ultrafiltration membrance filter;
(C) membrane concentration liquid after ethanol sedimentation gets Crude polysaccharides, deproteinated again through ethanol sedimentation, dry tea polysaccharide;
(D) film sees through liquid through the separation and purification of second resin adsorption chromatography, produces tea-polyphenol by-product trimethyl-xanthine.
Used enzyme is the prozyme of cellulase and polygalacturonase in the complex enzyme hydrolysis extraction step, cellulase accounts for the 60-80% of prozyme dry weight, the weight ratio of tealeaves and water is 1: 10-30, the enzyme add-on is the 0.05-0.25% of dry weight of tea leaves, extraction time 40-80 minute, temperature 40-60 ℃, pH value scope 4.0-6.0.
Filter residue after complex enzyme hydrolysis has extracted adds water to be continued to extract, and the weight ratio of tealeaves and water is 1: 10-20, extraction time 20-40 minute, temperature 40-60 ℃, pH value scope 4.0-7.0.
Ultrafiltration membrance filter uses the ultra-filtration membrane of molecular weight cut-off as 30kD-60kD.
In the second resin adsorption chromatography separating step, the first step use to tea-polyphenol have higher absorption and wash-out optionally acrylic acid series macroporous adsorbent resin A (hereinafter to be referred as the A resin) post adsorption chromatography produce tea-polyphenol, use the second stage has polystyrene macroporous adsorbent resin B (hereinafter to be referred as the B resin) the post absorption that higher absorption selects to trimethyl-xanthine and reclaims trimethyl-xanthine and regenerated acidic eluent.
The acrylic acid series macroporous adsorbent resin can be XAD7 or HP
2MG etc.
The polystyrene macroporous adsorbent resin can be XAD4, XAD16, XAD1600, HPD500, NKA-2, LSA5 or AB-8 etc.
It is that A resin column on the extracting solution behind the ultrafiltration membrance filter is adsorbed that first step resin column adsorption chromatography is produced tea-polyphenol, the absorption back is earlier with acid eluent wash-out trimethyl-xanthine, use the aqueous ethanolic solution wash-out tea-polyphenol of 50%-95% again, ethanol eluate is through reclaiming ethanol, the dry tea-polyphenol product that gets.
It is with B resin column absorption trimethyl-xanthine on the acid elutriant of A resin that trimethyl-xanthine is reclaimed in second stage resin column absorption, seeing through liquid is the acid eluent of regenerated, B resin after the absorption aqueous ethanolic solution wash-out of 50%-95%, elutriant reclaims ethanol, the dry thick product of trimethyl-xanthine that gets, and further available crystallization or subliming method are made with extra care trimethyl-xanthine.
Acid eluent is sulfuric acid or the hydrochloric acid soln that contains 0-30% alcoholic acid 3-10%.
Because the main component of tealeaves cell walls is a Mierocrystalline cellulose, so prozyme is based on cellulase, and polygalacturonase content is less, and cellulase accounts for the 60-80% of prozyme dry weight, can reach ideal enzymolysis broken wall, improves the effect of effective component extraction rate.
Tea polysaccharide is a class and protein bound acidic polysaccharose or acid glycoprotein together, mainly exist with glycopeptide or glycoprotein form, the mixed polysaccharide that its polysaccharide partly is made up of different monose, the main monose of forming has semi-lactosi, glucose, pectinose, wood sugar, Fucose etc.The relative molecular mass of tea polysaccharide, polysaccharide protein is generally between 40kD-100kD.Therefore, the ultra-filtration membrane with 30kD-60kD can remove macromolecular substance such as tea polysaccharide in the extracting solution and tea albumen.The present invention will reclaim polysaccharide, avoid resin stain and the three that improves the quality of products organically combines by ultra-filtration process.
The present invention filters out from a large amount of resins tea-polyphenol, trimethyl-xanthine absorption and the excellent acrylic acid series macroporous adsorbent resin A of wash-out selectivity, adopt two stepwise elution chromatographic technique separating tea multi-phenols, trimethyl-xanthine, selection elutes trimethyl-xanthine earlier the very low acid eluent of the eluting rate of tea-polyphenol, then uses the ethanol elution tea-polyphenol again.With another polystyrene macroporous adsorbent resin B that trimethyl-xanthine is had highly selective, the trimethyl-xanthine in the A resin column fs elutriant is reclaimed in absorption, but by-product trimethyl-xanthine not only, and make this elutriant obtain regeneration and recycle simultaneously, so constitute complete second resin method separation and purification tea-polyphenol, trimethyl-xanthine novel process, avoided the use of noxious solvent and Harmful chemicals fully.
The present invention belongs to weakly alkaline and the characteristics of tea-polyphenol meta-acid according to trimethyl-xanthine, to having optionally A resin of excellent wash-out, with the stepwise elution agent of acidic ethanol as the wash-out trimethyl-xanthine.Along with the increase of alcohol concn in the eluent and the reduction of acid concentration, the eluting rate of trimethyl-xanthine and tea-polyphenol increases, and the selectivity of wash-out reduces, though can reduce the wash-out loss that the consumption of eluent has increased tea-polyphenol.Therefore, acid eluent consists of sulfuric acid or the hydrochloric acid soln that contains 0-30% alcoholic acid 3-10%.
Advantage of the present invention:
(1) effective constituent at tealeaves all is in the protoplastis, and protoplastis is in the characteristics under cell walls and the intercellular substance parcel, selecting main component for use is that the prozyme liquid of cellulase and polygalacturonase take to divide Mierocrystalline cellulose, hemicellulose and the pectin substance that is deconstructed into cell walls and intercellular substance, make cell walls and intercellular substance structure produce variations such as the part is loose, expansion, collapse, thereby increased the diffusion area of effective constituent, reduce resistance to mass transfer, improved extraction ratio of effective constituents, more remarkable for its effect of macromolecular tea polysaccharide.The tea-polyphenol extraction yield is up to more than 98%, and the trimethyl-xanthine extraction yield can reach about 88%, and the tea polysaccharide yield is that 2%-3% is 2-3 times with water extraction tea polysaccharide yield under the condition.
(2) because of the remarkable broken wall effect of enzymolysis, extract raw material tealeaves and can not pulverize, simplified technology, also help the filtration of tea grounds.
(3) the effect specificity of enzyme is strong, and the molecular structure of effective constituent is not had influence.Enzyme is put forward process and can be carried out at low temperatures, because the main active ingredient one catechin oxidational losses of the low tea-polyphenol of temperature is few, energy consumption is low, in the tea-polyphenol that enzymolysis process extracts the catechin relative content than boiling water extraction exceed 9%～10%, the biological activity of the tea polysaccharide of extract at low temperature is also stronger.
(4) ultrafiltration membrance filter extracting solution, made things convenient on the one hand to reclaim the very tea polysaccharide of high value has been arranged, removed extracting solution behind the impurity such as polysaccharide, albumen in addition and can avoid pollution, improved the life cycle of adsorption chromatography post greatly, and make the purity of tea-polyphenol product improve 5%-8% resin.
(5) the present invention uses tea-polyphenol is had optionally macroporous adsorbent resin A and trimethyl-xanthine had the macroporous adsorbent resin B of highly selective of excellent absorption and wash-out, forms second resin method separating tea multi-phenol, trimethyl-xanthine technology.Solved the caffein-free difficult problem during the resin method tea-polyphenol is produced, process is simple, quality product reaches the first grade standard.And, only use alcohol to be solvent, production safety, health, environmental friendliness, that product does not have hazardous solvent is residual, helps the application at field of food.
(6) technology of the present invention, the front and back operation forms organic whole, can produce tea-polyphenol, trimethyl-xanthine, three kinds of products of tea polysaccharide, and tea raw material is fully utilized.Good product quality, yield height, the purity of product tea-polyphenol＞90%, trimethyl-xanthine＜4%, yield＞10%; The purity of trimethyl-xanthine＞95%, yield＞1%; The sugar degree of tea polysaccharide is＞50%, and yield accounts for the 2.0%-3.0% of dry weight of tea leaves.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Further elaborate the present invention below in conjunction with accompanying drawing.
A kind of processing method of from tealeaves, extracting tea-polyphenol by-product trimethyl-xanthine and tea polysaccharide, technical process is as follows:
1) tealeaves need not pulverized, and adds water 10-30 doubly, is warmed up to 40-60 ℃, adjust pH scope 4.0-6.0, and adding the prozyme liquid measure is 0.05-0.25%, extraction time 40-80 minute.Tea grounds after the filtration adds water 10-20 doubly, and temperature 40-60 ℃, pH value scope 4.0-7.0 extracted 20-40 minute.
2) merge twice extracting solution, with the ultrafiltration membrance filter of molecular weight cut-off 30kD-60kD, membrane concentration liquid gets thick tea polysaccharide through ethanol sedimentation, and the water dissolution Crude polysaccharides is after the precipitation method deproteinated, again through alcohol precipitation, washing, dry tea polysaccharide.
3) film sees through A resin column Adsorption of Tea Polyphenols, trimethyl-xanthine on the liquid, and the resin column after the absorption is wash-out trimethyl-xanthine and tea-polyphenol in two stages.Fs is with acid eluent wash-out trimethyl-xanthine, and subordinate phase is with the aqueous ethanolic solution wash-out tea-polyphenol of 50%-95%, and elutriant is through reclaiming ethanol, dry tea-polyphenol product.
4) B resin column absorption trimethyl-xanthine on the acid elutriant of A resin, seeing through liquid is the restored acid eluent, can be recycled.With the B resin after the aqueous ethanolic solution wash-out absorption of 50%-95%, elutriant reclaims ethanol, and the dry thick product of trimethyl-xanthine that gets is again with crystallization or the refining trimethyl-xanthine of subliming method.
The Crude polysaccharides deproteinated, used precipitating agent is a trichloroacetic acid solution, and wherein the concentration of trichoroacetic acid(TCA) is 2-10%, and dosage is 1/10 of a polysaccharide soln.
In the present invention, described refining trimethyl-xanthine method, available crystallization or subliming method.
In the present invention, described process water can be distilled water or deionized water.
In the present invention, described aqueous ethanolic solution, available edible ethanol preparation.
In the present invention, described drying can be vacuum-drying, lyophilize, spraying drying.
Embodiment:
Embodiment 1:
1) tealeaves 1kg adds water 20L, is warmed up to 40 ℃, and adjust pH scope 4.5 adds prozyme liquid measure 0.8g, 60 minutes extraction times; Filter residue after the filtration adds water 15L, 60 ℃ of temperature, and pH value 6 was extracted 40 minutes.
2) merge twice extracting solution, with molecular weight cut-off is the polysulfone hollow fibre ultrafiltration membrance filter of 30kD, membrane concentration liquid gets thick tea polysaccharide through ethanol sedimentation, behind the water dissolution Crude polysaccharides, drip the trichloroacetic acid precipitation albumen of 1/10 volume, 3% concentration, the filtrate behind the filtration albumen is again through alcohol precipitation, filtration, washing, the dry tea polysaccharide that gets.The sugar degree of tea polysaccharide is 50.5%, and yield accounts for 2.5% of dry weight of tea leaves.
3) film sees through XAD7 resin column Adsorption of Tea Polyphenols, trimethyl-xanthine on the liquid.Resin column after the absorption, fs is used 5% ethanol and the 5% vitriolic acidic solution wash-out trimethyl-xanthine of 8BV (the BV value is the resin bed volume), subordinate phase is with 95% the aqueous ethanolic solution wash-out tea-polyphenol of 4BV, elutriant through reclaim ethanol, lyophilize gets the tea-polyphenol product.The purity 94.3% of product tea-polyphenol, yield 13%.
4) AB-8 resin column absorption trimethyl-xanthine on the sour elutriant of XAD7 resin, seeing through liquid is the restored acid eluent, can be recycled, with the B resin after the 95% aqueous ethanolic solution wash-out absorption of 3.5BV, elutriant reclaims ethanol, vacuum-drying gets the thick product of trimethyl-xanthine, again with the refining trimethyl-xanthine of subliming method.The purity 97.5% of trimethyl-xanthine, yield 1.2%.
Embodiment 2:
1) tealeaves 1kg adds water 30L, is warmed up to 50 ℃, and adjust pH 5.5 adds prozyme liquid measure 2.0g, 70 minutes extraction times.Filter residue after the filtration adds water 10L, 50 ℃ of temperature, and pH value 6 was extracted 30 minutes.
2) merge twice extracting solution, with molecular weight cut-off is the polysulfone hollow fibre ultrafiltration membrance filter of 50kD, membrane concentration liquid gets thick tea polysaccharide through ethanol sedimentation, the trichloroacetic acid precipitation deproteinated that adds 1/10 volume, 5% concentration behind the water dissolution Crude polysaccharides, filtrate filtered are again through alcohol precipitation, filtration, washing, the dry tea polysaccharide that gets.The sugar degree of tea polysaccharide is 53.2%, and yield accounts for dry weight of tea leaves 2.4%.
3) film sees through HP on the liquid
2MG resin column Adsorption of Tea Polyphenols, trimethyl-xanthine, resin column after the absorption, the fs, as acid eluent wash-out trimethyl-xanthine, subordinate phase was with 85% the aqueous ethanolic solution wash-out tea-polyphenol of 4BV with 8% the hydrochloric acid soln of 5BV, elutriant is through reclaiming ethanol, and lyophilize gets the tea-polyphenol product.The purity 96.2% of product tea-polyphenol, yield 11%.
4) HP
2XAD4 resin column absorption trimethyl-xanthine on the acid elutriant of MG resin, seeing through liquid is the restored acid eluent, can be recycled.With the XAD4 resin after 85% the aqueous ethanolic solution wash-out absorption of 4BV, elutriant reclaims ethanol, vacuum-drying gets the thick product of trimethyl-xanthine, again with the refining trimethyl-xanthine of subliming method.The purity 95% of trimethyl-xanthine, yield 1.3%.
Claims (10)
1. processing method of from tealeaves, extracting tea-polyphenol by-product trimethyl-xanthine and tea polysaccharide, its steps in sequence is as follows:
(A) effective constituents such as tea-polyphenol, trimethyl-xanthine and tea polysaccharide in extraction of employing complex enzyme hydrolysis and the water extraction tealeaves;
(B) extracting solution is through ultrafiltration membrance filter;
(C) membrane concentration liquid after ethanol sedimentation gets Crude polysaccharides, deproteinated again through ethanol sedimentation, dry tea polysaccharide;
(D) film sees through liquid through the separation and purification of second resin adsorption chromatography, produces tea-polyphenol by-product trimethyl-xanthine.
2. the processing method of extraction tea-polyphenol by-product trimethyl-xanthine according to claim 1 and tea polysaccharide, it is characterized in that used enzyme is the prozyme of cellulase and polygalacturonase in the complex enzyme hydrolysis extraction step, cellulase accounts for the 60-80% of prozyme dry weight, the weight ratio of tealeaves and water is 1: 10-30, the enzyme add-on is the 0.05-0.25% of dry weight of tea leaves, extraction time 40-80 minute, temperature 40-60 ℃, pH value scope 4.0-6.0.
3. the processing method of extraction tea-polyphenol by-product trimethyl-xanthine according to claim 1 and 2 and tea polysaccharide, it is characterized in that the filter residue after complex enzyme hydrolysis has extracted adds water continuation extraction, the weight ratio of tealeaves and water is 1: 10-20, extraction time 20-40 minute, temperature 40-60 ℃, pH value scope 4.0-7.0.
4. the processing method of extraction tea-polyphenol by-product trimethyl-xanthine according to claim 1 and tea polysaccharide is characterized in that ultrafiltration membrance filter uses the ultra-filtration membrane of molecular weight cut-off as 30kD-60kD.
5. the processing method of extraction tea-polyphenol by-product trimethyl-xanthine according to claim 1 and tea polysaccharide, it is characterized in that in the second resin adsorption chromatography separating step, the first step use to tea-polyphenol have higher absorption and wash-out optionally acrylic acid series macroporous adsorbent resin A post adsorption chromatography produce tea-polyphenol, use the second stage has the polystyrene macroporous adsorbent resin B post absorption that higher absorption selects to trimethyl-xanthine and reclaims trimethyl-xanthine and regenerated acidic eluent.
6. the processing method of extraction tea-polyphenol by-product trimethyl-xanthine according to claim 5 and tea polysaccharide is characterized in that the acrylic acid series macroporous adsorbent resin can be XAD7 or HP
2MG.
7. the processing method of extraction tea-polyphenol by-product trimethyl-xanthine according to claim 5 and tea polysaccharide is characterized in that the polystyrene macroporous adsorbent resin can be XAD4, XAD16, XAD1600, HPD500, NKA-2, LSA5 or AB-8.
8. the processing method of extraction tea-polyphenol by-product trimethyl-xanthine according to claim 5 and tea polysaccharide, it is characterized in that it is that A resin column on the extracting solution behind the ultrafiltration membrance filter is adsorbed that first step resin column adsorption chromatography is produced tea-polyphenol, the absorption back is earlier with acid eluent wash-out trimethyl-xanthine, use the aqueous ethanolic solution wash-out tea-polyphenol of 50%-95% again, ethanol eluate is through reclaiming ethanol, the dry tea-polyphenol product that gets.
The processing method of 9 extraction tea-polyphenol by-product trimethyl-xanthines according to claim 5 and tea polysaccharide, it is characterized in that it is with B resin column absorption trimethyl-xanthine on the acid elutriant of A resin that trimethyl-xanthine is reclaimed in second stage resin column absorption, seeing through liquid is the acid eluent of regenerated, B resin after the absorption aqueous ethanolic solution wash-out of 50%-95%, elutriant reclaims ethanol, the dry thick product of trimethyl-xanthine that gets, and further available crystallization or subliming method are made with extra care trimethyl-xanthine.
10, according to the processing method of one of any described extraction tea-polyphenol by-product trimethyl-xanthine of claim 6-9 and tea polysaccharide, it is characterized in that acid eluent is sulfuric acid or the hydrochloric acid soln that contains 0-30% alcoholic acid 3-10%.
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