CN102875691A - Method for synchronously preparing active substances from tea dregs - Google Patents
Method for synchronously preparing active substances from tea dregs Download PDFInfo
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Abstract
A method for synchronously preparing active substances from tea dregs belongs to a production method of chemicals or drugs and solves the problems of high consumption of organic reagents, high process cost, low yield, low separating efficiency, low utilization rate of raw materials and the like in the existing purification and preparation methods. The method includes the steps of removing impure proteins, precipitating polysaccharide, separating twice by silica gel dry column and the like. Specific protein precipitant and polysaccharide precipitant are used, so that consumption of organic reagents is reduced greatly, production cycle and cost are reduced, and environment can be protected. The twice separation process using silica gel dry column has the advantages that at most one column volume of solvent is consumed, column hold-up is low and the like, so that separating efficiency is improved greatly, and separating cost is reduced. Monomers with more than 95% in purity such as EGCG (epigallocatechin gallate), EGC (epigallocatechin) and ECG (epicatechin gallate) are obtained while tea polysaccharide, caffeine and tea Polyphenols are obtained. The method is simple and feasible and convenient for industrial production.
Description
Technical field
The invention belongs to the manufacture method of chemical substance or medicine, the tea grounds that is specifically related to be discarded in the Tea Production process obtains the method for tea polysaccharide, trimethyl-xanthine, tea-polyphenol, EGCG, EGC, ECG isoreactivity material synchronously as raw material.
Background technology
Tea is state's drink of China, also be a kind of drink in the pink of condition, and China is universally acknowledged tealeaves country of origin.Contain the organic chemistry composition in the tealeaves and reach kind more than 450, inorganic mineral element reaches kind more than 40.Organic chemical composition in the tealeaves and inorganic mineral element contain many nutritive ingredients and effective component.Organic chemical composition mainly contains: tea polyphenols, vegeto-alkali, protein, amino acid, VITAMIN, pectin element, organic acid, lipopolysaccharides, carbohydrate, enzyme, pigment etc.And at present, generally believe that the main composition in the tealeaves is tea-polyphenol, tea polysaccharide and trimethyl-xanthine etc.
Tea-polyphenol has another name called tea tannin, tea tannin, is the general name of polyhydroxyl phenolic compound contained in the tealeaves, referred to as TP.Its main component is catechin (flavanol compound), flavones, flavonols, anthocyan, phenolic acid, depside and polymerization phenols etc.Wherein catechin compounds is the main body composition of tea-polyphenol, accounts for 65%～80% of tea-polyphenol total amount.Catechin compounds mainly comprises: the materials such as NVP-XAA 723 (EGCG), epigallocatechin (EGC), L-Epicatechin gallate (ECG), wherein, the content of EGCG is the highest and be concerned most.
EGCG is a kind of composition that extracts from Chinese green tea, it is the main activity of green tea and water-soluble components, it is the highest component of content in the catechin, account for the 9%-13% of green tea gross weight, because have special stereochemical structure, EGCG has very strong anti-oxidant activity, is taking on important role aspect anticancer and the cardiovascular disorder.In addition, it is also as the reversal agent of multi-drug resistance of the tumor, can improve cancer cells to the susceptibility of chemotherapy and alleviate toxicity to heart.Many EGCG of studies show that have Green Tea Extract DNA infringement, radioprotective and ultraviolet ray, stop oil peroxidation, reduce the content of low density cholesterol, extremely-low density cholesterol and triglyceride level in the serum, the signal transmission that interfere with cancer cells existence is required, suppress the carcinogenic substance in the diet, the vigor that jointly stops some carcinogenic substance with other enzymes in intestines, liver and the lung and antioxidant action, remove free radical, resist the impact of pollution, Exposure to Sunlight and smoking, control skin aging and the multiple efficacies such as wrinkling.
The tea polysaccharide that is rich in the tealeaves is a kind of acid glycoprotein, and is combined with a large amount of mineral elements, is called the Tea Polysaccharides mixture, referred to as Tea Polysaccharides or tea polysaccharide (Tea Polysaccharide).It is that protein part mainly is comprised of about 20 kinds of common amino acid, the part of sugar is mainly by pectinose, wood sugar, Fucose, glucose, semi-lactosi etc., mineral element is mainly by calcium, magnesium, iron, manganese etc. and a small amount of trace element, such as compositions such as rare earth elements.Have the effects such as hypoglycemic, reducing blood-fat, strengthening immunity, hypotensive, reducing heart rate, increase coronary flow, anticoagulation, antithrombotic and hypoxia tolerance, the discovered in recent years tea polysaccharide also has the effect for the treatment of diabetes.
Trimethyl-xanthine claims again caffeine, is a kind of xanthine alkaloid compound, is a kind of central nervous excitation agent, can be temporary transient drive away sleepiness and regain one's vigor.Have coffee, tea, soft drink and the energy drink of caffeine composition in very great demand, therefore, caffeine also is the psychotropic substances that the most generally are used in the world.In the North America, 90% grownup uses caffeine every day.It moderately uses the effect of dispelling fatigue, excitor nerve, is used for the treatment of clinically neurasthenia and stupor recovery.
At present, very huge at China's Tea planting and processing industry thereof, China's sales of tea volume had been broken through 15,000,000,000 yuan in 2004.In the Tea Industry development, it should be noted that the tea grounds (tankage) that produces in a large amount of Tea Processing processes does not utilize fully.At present for tea grounds, mainly for the production of the teabag of low side, tea cake, compost etc., in recent years, the further deep processing of manufacturer is arranged also, utilize tea grounds to produce tea-polyphenol.The present invention obtains tea polysaccharide, trimethyl-xanthine, tea-polyphenol synchronously take tea grounds as raw material, and can obtain the higher high purity EGCG of added value, the monomer components such as EGC, ECG, has greatly improved value-added content of product when improving resource utilization.
At present, separate the open report that obtains active substance for extraction from tealeaves more, but all have certain deficiency, for example:
Xie Yu equals to be called in patent No. ZL200810107066, name in 2008 the method for Simultaneous Extraction of Tea Polyphenols and trimethyl-xanthine " a kind of from tealeaves ", the method is by boiling water lixiviate, sedimentation and filtration, extraction, drying and other steps, obtain simultaneously tea-polyphenol and trimethyl-xanthine, but the extracting process that the method adopts has not only increased production energy consumption and facility investment greatly, the extensive application of the organic reagents such as ethyl acetate is unfavorable for safety in production and environmental protection, and the tea-polyphenol purity that obtains is not high, does not obtain the products such as the higher tea polysaccharide of added value, EGCG;
Chen Haixia equals to be called in patent No. ZL200910068255, name in 2009 " a kind of method of extracting tea polysaccharide and tea-polyphenol from thick old green tea ", the steps such as the method adopts extrusion process, deionized water extraction, concentrates, ethanol precipitation, separation, vacuum lyophilization.The advantage of the method is to adopt single-screw extrusion machine under suitable moisture and temperature condition raw material to be pushed, so that raw material is carried out pre-treatment, improved extraction efficiency, but the polysaccharide ethanol precipitation that the method adopts inevitably consumes a large amount of organic reagents, and the product purity that obtains is not high, and added value is lower;
Li Qifeng was called " a kind of mechanochemistry principle of utilizing is simultaneously from the novel method of Extraction of Caffeine From Tea, tea-polyphenol and tea polysaccharide " in application number 200910095072, name in 2009, the method is by adding the powder of milling in tealeaves, to increase extraction efficiency, and the products such as tea-polyphenol, trimethyl-xanthine, tea polysaccharide have been obtained simultaneously, but the method has adopted the method for ethanol precipitation equally, and product purity is lower;
King's equality was called " a kind of method of extracting tea-polyphenol and separating monomer EGCG from tealeaves " in patent No. ZL200810059567, name in 2008, the method is with tealeaves and solid phase alkali reagent, jointly be ground, use water dissolution, stir, centrifugal, get supernatant liquor, produce precipitation after regulating pH, filter, obtaining filter residue is monomer EGCG; Gained filtrate is tea-polyphenol solution, and drying obtains the crude product tea-polyphenol.But the solid phase alkali reagent that the method is used has certain impact to environment, and the product that obtains is few, and tea-polyphenol purity is low, and raw-material utilization ratio is low;
Zhang Shouzheng was called " method of extracting tea-polyphenol, theanine, tea polysaccharide, tea pigment from tealeaves " in 2008 in patent No. ZL200610055145, name, although the method has obtained the various active material simultaneously, but in the technology that adopts: the technology such as constant temperature continuous countercurrent stage extraction, micro-filtration, ultrafiltration, reverse osmosis, CO2 supercritical extraction, but the fixed investment of these Technology Needs is large, production cost is high, is difficult to suitability for industrialized production.
Wang Junwei was called " a kind of method for batch production, separation and purification of catechin monomers EGCG " in 2009 in application number 200910273058, name, although the method has obtained highly purified EGCG monomer, but the reverse C18 filler that the method adopts separates, and has greatly increased production cost.
The tea grounds that the present invention is discarded in the Tea Production process discloses a kind of method that obtains synchronously tea polysaccharide, trimethyl-xanthine, tea-polyphenol, EGCG, EGC, ECG isoreactivity material as raw material.Specific protein precipitant and polysaccharide precipitation agent are adopted in invention, compare with traditional Sevage and remove protein method and ethanol precipitation polysaccharide method, greatly reduce expending of organic reagent, have saved production cycle and cost, and have been beneficial to protection of the environment.The method that the dried post of the secondary silica gel that invention is adopted separates, keep the advantages such as little owing to having the solvent and the post that expend at most a column volume, than methods such as traditional silicagel column separation, membrane filtration, reverse C18 filler separation, greatly promoted separation efficiency, save separation costs, and when obtaining tea polysaccharide, trimethyl-xanthine, tea-polyphenol, obtained purity greater than monomer components such as 95% EGCG, EGC, ECG.Simple process is easily gone, and is beneficial to suitability for industrialized production.
Summary of the invention
The invention provides a kind of from tea grounds the method for the standby various active material of interlock system, solve the problems such as the organic reagent usage quantity is large among existing separation and purification and the preparation method, process costs is high, yield is lower, separation efficiency is low, raw material availability is lower.
Of the present invention a kind of from tea grounds the method for the standby various active material of interlock system, comprising:
Except the foreign protein step; Get the tea grounds of being discarded in the Tea Production process, 70～100 ℃ of water extraction 2～4 times, add the volume of water and the mass ratio of tea grounds is 5: 1～15: 1 (V/W), filter behind the united extraction liquid, filtrate adds protein precipitant, foreign protein is removed in precipitin reaction, obtains tea grounds Deproteinization extracting solution after the centrifugal removal precipitation;
The polysaccharide precipitation step; With the tea grounds Deproteinization extracting solution that obtains, add the polysaccharide precipitation agent, adjust pH6.0～9.0, react after 4～12 hours, with after dehydrated alcohol, acetone, the ether agitator treating precipitation, drying obtains tea polysaccharide successively for centrifugal being precipitated respectively and supernatant liquor, gained precipitation; The supernatant liquor of gained is evaporated to driedly, obtains tea grounds and removes polyoses extract;
The dried post separating step of the silica gel first time; The tea grounds that obtains is removed polyoses extract, be splined on the dried post of silica gel, it is 1/80～1/300 that tea grounds removes the mass ratio of polyoses extract and silica gel based filler, utilizes pressure difference with the developping agent descending development under normal pressure, obtains respectively trimethyl-xanthine and tea-polyphenol; Developping agent is the mixed solution of methyl alcohol and normal hexane or the mixed solution of methyl alcohol and ethyl acetate;
The dried post separating step of the silica gel second time; With the tea-polyphenol that obtains, be splined on the dried post of silica gel, the mass ratio of tea-polyphenol and silica gel based filler is 1/50～1/200, under normal pressure, utilize pressure difference with the developping agent descending development, obtain respectively purity greater than 95% NVP-XAA 723 (EGCG), epigallocatechin (EGC), L-Epicatechin gallate (ECG); Developping agent is the mixed solution of dehydrated alcohol and normal hexane or the mixed solution of dehydrated alcohol and acetone;
Described except in the foreign protein step, described protein precipitant is: Freon 113 or 2～5% the Tricholroacetic Acid aqueous solution (V/V); Foreign protein is removed in described precipitin reaction, its process is: add Freon 113 in filtrate, adding Freon 113 is 1: 2～2: 1 (V/V) with the filtrate volume ratio, stirring reaction 10～20min, after the centrifugal removal precipitation, the water intaking layer obtains tea grounds Deproteinization extracting solution liquid; Or in filtrate, drip 2～5% the Tricholroacetic Acid aqueous solution, and adding the Tricholroacetic Acid aqueous solution is 1: 10～1: 20 (V/V) with the filtrate volume ratio, 5～10 ℃ left standstill 8～16 hours, obtained tea grounds Deproteinization extracting solution after the centrifugal removal precipitation.
In the described polysaccharide precipitation step, described polysaccharide precipitation agent is: a kind of in 0.05g/ml cetyltrimethylammonium hydroxide Trimethylamine 99 bromide (CTA-OH) aqueous solution, 0.05g/ml cetyl pyridinium (CP-OH) aqueous solution, the volume ratio of polysaccharide precipitation agent and tea grounds Deproteinization extracting solution is 0.05: 1～0.2: 1 (V/V).
In the dried post separating step of the described silica gel first time and the dried post separating step of the silica gel second time:
The dried post of described silica gel is for to be filled with silica gel based filler, 5: 1～20: 1 separation column devices of aspect ratio, and the silica gel based filler is comprised of silica gel and diatomite, and the mass percent of diatomite and silica gel based filler is 5%～20%; The silica gel particle diameter is 30 μ m～80 μ m, and the silica gel activity is II～III level; The process of dry column-packing that the filling process of the dried post of described silica gel and general post separate employing is consistent.
In the dried post separating step of the described silica gel first time:
The volume ratio of described developping agent is: methyl alcohol: normal hexane=1: 2～5: 1 (V/V), perhaps methyl alcohol: ethyl acetate=1: 3～4: 1 (V/V);
The process of described descending development is: after the loading, developping agent is added from the dried capital of silica gel, utilize the pressure difference descending development under normal pressure, when developer flow to silica gel is done the column bottom, stop the exhibition layer; After the silica gel based filler that is rich in respectively trimethyl-xanthine and tea-polyphenol scraped from the dried post of silica gel, add 95% ethanol, vibration wash-out 10～20 minutes or ultrasonic wash-out are 5～15 minutes on shaking table, repeat wash-out 2～4 times, with the elutriant decompression that obtains
Evaporate to dryness namely obtains respectively trimethyl-xanthine and tea-polyphenol; The described silica gel based filler that is rich in respectively trimethyl-xanthine and tea-polyphenol, its residing position in the dried post of silica gel are the target product Rf value R that obtains with reference to silica gel thin-layer experiment under the identical developping agent condition
fDetermine.
In the dried post separating step of the described silica gel second time:
The volume ratio of described developping agent is: dehydrated alcohol: normal hexane=8: 1～95: 5 (V/V), perhaps dehydrated alcohol: acetone=7: 1～9: 1 (V/V);
The process of described descending development is: after the loading, developping agent is added from the dried capital of silica gel, utilize the pressure difference descending development under normal pressure, when developer flow to silica gel is done the column bottom, stop the exhibition layer; After the silica gel based filler that is rich in respectively EGCG, EGC, ECG scraped from the dried post of silica gel, add 95% ethanol, vibration wash-out 10～20 minutes or ultrasonic wash-out are 5～15 minutes on shaking table, repeat wash-out 2～4 times, with the elutriant evaporated under reduced pressure that obtains, namely obtain respectively purity greater than 95% EGCG, EGC, ECG; The described silica gel based filler that is rich in respectively EGCG, EGC, ECG, its residing position in the dried post of silica gel are the target product Rf value R that obtains with reference to silica gel thin-layer experiment under the identical developping agent condition
fDetermine.
Embodiment
Embodiment 1
(1) except the foreign protein step: get the tea grounds 100g that is discarded in the Tea Production process, add water 1500ml, add the volume of water and the mass ratio of tea grounds is 15: 1 (V/W), after extracting 3 times under 70 ℃, filter behind the united extraction liquid, get filtrate 4200ml, in filtrate, add the 2100ml Freon 113 as protein precipitant, adding Freon 113 is 1: 2 (V/V) with the filtrate volume ratio, stirring reaction 20min, after the centrifugal removal precipitation, the water intaking layer obtains tea grounds Deproteinization extracting solution 4150ml.
(2) polysaccharide precipitation step: the tea grounds Deproteinization extracting solution 4150ml that step (1) is obtained, cetyltrimethylammonium hydroxide Trimethylamine 99 bromide (CTA-OH) aqueous solution that adds 415ml0.05g/ml, wherein, the volume ratio of polysaccharide precipitation agent and tea grounds Deproteinization extracting solution is 0.1: 1 (V/V), adjust pH7.5, react after 8 hours centrifugal being precipitated, with after dehydrated alcohol, acetone, the ether agitator treating precipitation, drying obtains tea polysaccharide 4.37g to precipitation successively.The supernatant liquor of centrifugal gained is evaporated to driedly, obtains tea grounds and removes polyoses extract 32.50g;
(3) the dried post separating step of the silica gel first time: the III level activated silica gel of getting 4387.50g, particle diameter 50 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 10%) of interpolation 487.50g, dry column-packing after mixing gets the post aspect ratio and is 5: 1 the dried post of silica gel; The tea grounds that step (2) is obtained goes polyoses extract 32.50g dry method to be splined on the dried post of silica gel, it is 1/150 that tea grounds removes the mass ratio of polyoses extract and silica gel based filler, under normal pressure, utilize pressure difference, take methyl alcohol: normal hexane=1: 2 (V/V) is as the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of trimethyl-xanthine and tea-polyphenol under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively trimethyl-xanthine and tea-polyphenol scrapes from the dried post of silica gel, add 95% ethanol, the vibration wash-out is 20 minutes on shaking table, repeats wash-out 2 times, with the elutriant evaporated under reduced pressure that obtains, obtain respectively trimethyl-xanthine 3.95g and tea-polyphenol 12.20g
(4) the dried post separating step of the silica gel second time: the III level activated silica gel of getting 1098.00g, particle diameter 50 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 10%) of interpolation 122.00g, dry column-packing after mixing gets the post aspect ratio and is 5: 1 the dried post of silica gel; The tea-polyphenol 12.20g dry method that step (3) is obtained is splined on the dried post of silica gel, the mass ratio of tea-polyphenol and silica gel based filler is 1/100, under normal pressure, utilize pressure difference, take dehydrated alcohol: normal hexane=8: 1 (V/V) is as the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of EGCG, EGC, ECG under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively EGCG, EGC, ECG scrapes from the dried post of silica gel, add 95% ethanol, the vibration wash-out is 20 minutes on shaking table, repeats wash-out 2 times, elutriant evaporated under reduced pressure with obtaining obtains respectively trimethyl-xanthine EGCG6.13g, EGC1.77g, ECG1.06g.
Embodiment 2
(1) except the foreign protein step: get the tea grounds 50g that is discarded in the Tea Production process, add water 500ml, add the volume of water and the mass ratio of tea grounds is 10: 1 (V/W), after extracting 2 times under 100 ℃, filter behind the united extraction liquid, get filtrate 910ml, in filtrate, add the 1820ml Freon 113 as protein precipitant, adding Freon 113 is 2: 1 (V/V) with the filtrate volume ratio, stirring reaction 10min, after the centrifugal removal precipitation, the water intaking layer obtains tea grounds Deproteinization extracting solution 885ml.
(2) polysaccharide precipitation step: the tea grounds Deproteinization extracting solution 885ml that step (1) is obtained, cetyl pyridinium (CP-OH) aqueous solution that adds 177ml0.05g/ml, wherein, the volume ratio of polysaccharide precipitation agent and tea grounds Deproteinization extracting solution is 0.2: 1 (V/V), adjust pH9.0, react after 12 hours centrifugal being precipitated, with after dehydrated alcohol, acetone, the ether agitator treating precipitation, drying obtains tea polysaccharide 2.11g to precipitation successively.The supernatant liquor of centrifugal gained is evaporated to driedly, obtains tea grounds and removes polyoses extract 15.68g;
(3) the dried post separating step of the silica gel first time: the II level activated silica gel of getting 3763.20g, particle diameter 30 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 20%) of interpolation 940.80g, dry column-packing after mixing gets the post aspect ratio and is 10: 1 the dried post of silica gel; The tea grounds that step (2) is obtained goes polyoses extract 15.68g dry method to be splined on the dried post of silica gel, it is 1/300 that tea grounds removes the mass ratio of polyoses extract and silica gel based filler, under normal pressure, utilize pressure difference, take methyl alcohol: normal hexane=5: 1 (V/V) is as the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of trimethyl-xanthine and tea-polyphenol under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively trimethyl-xanthine and tea-polyphenol scrapes from the dried post of silica gel, add 95% ethanol, the vibration wash-out is 10 minutes on shaking table, repeats wash-out 4 times, with the elutriant evaporated under reduced pressure that obtains, obtain respectively trimethyl-xanthine 1.82g and tea-polyphenol 5.88g
(4) the dried post separating step of the silica gel second time: the II level activated silica gel of getting 940.80g, particle diameter 30 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 20%) of interpolation 235.20g, dry column-packing after mixing gets the post aspect ratio and is 10: 1 the dried post of silica gel; The tea-polyphenol 5.88g dry method that step (3) is obtained is splined on the dried post of silica gel, the mass ratio of tea-polyphenol and silica gel based filler is 1/200, under normal pressure, utilize pressure difference, take dehydrated alcohol: normal hexane=95: 5 (V/V) is as the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of EGCG, EGC, ECG under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively EGCG, EGC, ECG scrapes from the dried post of silica gel, add 95% ethanol, the vibration wash-out is 10 minutes on shaking table, repeats wash-out 4 times, elutriant evaporated under reduced pressure with obtaining obtains respectively trimethyl-xanthine EGCG2.99g, EGC0.81g, ECG0.42g.
Embodiment 3
(1) except the foreign protein step: get the tea grounds 25g that is discarded in the Tea Production process, add water 75ml, add the volume of water and the mass ratio of tea grounds is 5: 1 (V/W), after extracting 4 times under 85 ℃, filter behind the united extraction liquid, get filtrate 280ml, in filtrate, add the 280ml Freon 113 as protein precipitant, adding Freon 113 is 1: 1 (V/V) with the filtrate volume ratio, stirring reaction 15min, after the centrifugal removal precipitation, the water intaking layer obtains tea grounds Deproteinization extracting solution 266ml.
(2) polysaccharide precipitation step: the tea grounds Deproteinization extracting solution 266ml that step (1) is obtained, cetyltrimethylammonium hydroxide Trimethylamine 99 bromide (CTA-OH) aqueous solution that adds 39.90ml0.05g/ml, wherein, the volume ratio of polysaccharide precipitation agent and tea grounds Deproteinization extracting solution is 0.15: 1 (V/V), adjust pH6.0, react after 4 hours centrifugal being precipitated, with after dehydrated alcohol, acetone, the ether agitator treating precipitation, drying obtains tea polysaccharide 0.84g to precipitation successively.The supernatant liquor of centrifugal gained is evaporated to driedly, obtains tea grounds and removes polyoses extract 7.75g;
(3) the dried post separating step of the silica gel first time: the III level activated silica gel of getting 1472.50g, particle diameter 80 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 5%) of interpolation 77.50g, dry column-packing after mixing gets the post aspect ratio and is 20: 1 the dried post of silica gel; The tea grounds that step (2) is obtained goes polyoses extract 7.75g dry method to be splined on the dried post of silica gel, it is 1/200 that tea grounds removes the mass ratio of polyoses extract and silica gel based filler, under normal pressure, utilize pressure difference, take methyl alcohol: normal hexane=3: 1 (V/V) is as the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of trimethyl-xanthine and tea-polyphenol under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively trimethyl-xanthine and tea-polyphenol scrapes from the dried post of silica gel, add 95% ethanol, the vibration wash-out is 15 minutes on shaking table, repeats wash-out 3 times, with the elutriant evaporated under reduced pressure that obtains, obtain respectively trimethyl-xanthine 0.87g and tea-polyphenol 2.83g
(4) the dried post separating step of the silica gel second time: the III level activated silica gel of getting 134.42g, particle diameter 80 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 5%) of interpolation 7.08g, dry column-packing after mixing gets the post aspect ratio and is 20: 1 the dried post of silica gel; The tea-polyphenol 2.83g dry method that step (3) is obtained is splined on the dried post of silica gel, the mass ratio of tea-polyphenol and silica gel based filler is 1/50, under normal pressure, utilize pressure difference, take dehydrated alcohol: normal hexane=90: 10 (V/V) is as the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of EGCG, EGC, ECG under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively EGCG, EGC, ECG scrapes from the dried post of silica gel, add 95% ethanol, the vibration wash-out is 15 minutes on shaking table, repeats wash-out 3 times, elutriant evaporated under reduced pressure with obtaining obtains respectively trimethyl-xanthine EGCG1.39g, EGC0.44g, ECG0.31g.
Embodiment 4
(1) except the foreign protein step: get the tea grounds 200g that is discarded in the Tea Production process, add water 2000ml, add the volume of water and the mass ratio of tea grounds is 10: 1 (V/W), after extracting 3 times under 90 ℃, filter behind the united extraction liquid, get filtrate 5600ml, the Tricholroacetic Acid aqueous solution that in filtrate, adds 560ml2%, adding the Tricholroacetic Acid aqueous solution is 1: 10 (V/V) with the filtrate volume ratio, and 10 ℃ left standstill 8 hours, obtains tea grounds Deproteinization extracting solution 6100ml after the centrifugal removal precipitation.
(2) polysaccharide precipitation step: the tea grounds Deproteinization extracting solution 6100ml that step (1) is obtained, add 305ml0.05g/ml cetyl pyridinium (CP-OH) aqueous solution, wherein, the volume ratio of polysaccharide precipitation agent and tea grounds Deproteinization extracting solution is 0.05: 1 (V/V), adjust pH8.0, react after 10 hours centrifugal being precipitated, with after dehydrated alcohol, acetone, the ether agitator treating precipitation, drying obtains tea polysaccharide 8.61g to precipitation successively.The supernatant liquor of centrifugal gained is evaporated to driedly, obtains tea grounds and removes polyoses extract 63.75g;
(3) the dried post separating step of the silica gel first time: the III level activated silica gel of getting 4590.00g, particle diameter 50 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 10%) of interpolation 510.00g, dry column-packing after mixing gets the post aspect ratio and is 8: 1 the dried post of silica gel; The tea grounds that step (2) is obtained goes polyoses extract 63.75g dry method to be splined on the dried post of silica gel, it is 1/80 that tea grounds removes the mass ratio of polyoses extract and silica gel based filler, under normal pressure, utilize pressure difference, methyl alcohol: ethyl acetate=1: 3 (V/V) is the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of trimethyl-xanthine and tea-polyphenol under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively trimethyl-xanthine and tea-polyphenol scrapes, add 95% ethanol from the dried post of silica gel, in ultrasonic wash-out 15 minutes, repeat wash-out 2 times, with the elutriant evaporated under reduced pressure that obtains, obtain respectively trimethyl-xanthine 7.92g and tea-polyphenol 23.80g
(4) the dried post separating step of the silica gel second time: the III level activated silica gel of getting 3213.00g, particle diameter 50 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 10%) of interpolation 357.00g, dry column-packing after mixing gets the post aspect ratio and is 8: 1 the dried post of silica gel; The tea-polyphenol 23.80g dry method that step (3) is obtained is splined on the dried post of silica gel, the mass ratio of tea-polyphenol and silica gel based filler is 1/150, under normal pressure, utilize pressure difference, take dehydrated alcohol: acetone=7: 1 (V/V) is as the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of EGCG, EGC, ECG under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively EGCG, EGC, ECG scrapes from the dried post of silica gel, add 95% ethanol, in ultrasonic wash-out 15 minutes, repeat wash-out 2 times, elutriant evaporated under reduced pressure with obtaining obtains respectively trimethyl-xanthine EGCG11.89g, EGC3.41g, ECG1.74g.
Embodiment 5
(1) except the foreign protein step: get the tea grounds 300g that is discarded in the Tea Production process, add water 1500ml, add the volume of water and the mass ratio of tea grounds is 5: 1 (V/W), after extracting 3 times under 100 ℃, filter behind the united extraction liquid, get filtrate 4200ml, the Tricholroacetic Acid aqueous solution that in filtrate, adds 210ml5%, adding the Tricholroacetic Acid aqueous solution is 1: 20 (V/V) with the filtrate volume ratio, and 5 ℃ left standstill 16 hours, obtains tea grounds Deproteinization extracting solution 4350ml after the centrifugal removal precipitation.
(2) polysaccharide precipitation step: the tea grounds Deproteinization extracting solution 4350ml that step (1) is obtained, add 435ml0.05g/ml cetyltrimethylammonium hydroxide Trimethylamine 99 bromide (CTA-OH) aqueous solution, wherein, the volume ratio of polysaccharide precipitation agent and tea grounds Deproteinization extracting solution is 0.1: 1 (V/V), adjust pH9.0, react after 12 hours centrifugal being precipitated, with after dehydrated alcohol, acetone, the ether agitator treating precipitation, drying obtains tea polysaccharide 11.14g to precipitation successively.The supernatant liquor of centrifugal gained is evaporated to driedly, obtains tea grounds and removes polyoses extract 95.20g;
(3) the dried post separating step of the silica gel first time: the II level activated silica gel of getting 8568.00g, particle diameter 30 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 10%) of interpolation 952.00g, dry column-packing after mixing gets the post aspect ratio and is 20: 1 the dried post of silica gel; The tea grounds that step (2) is obtained goes polyoses extract 95.20g dry method to be splined on the dried post of silica gel, it is 1/100 that tea grounds removes the mass ratio of polyoses extract and silica gel based filler, under normal pressure, utilize pressure difference, methyl alcohol: ethyl acetate=4: 1 (V/V) is the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of trimethyl-xanthine and tea-polyphenol under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively trimethyl-xanthine and tea-polyphenol scrapes, add 95% ethanol from the dried post of silica gel, in ultrasonic wash-out 5 minutes, repeat wash-out 4 times, with the elutriant evaporated under reduced pressure that obtains, obtain respectively trimethyl-xanthine 11.93g and tea-polyphenol 36.00g
(4) the dried post separating step of the silica gel second time: the II level activated silica gel of getting 6480.00g, particle diameter 30 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 10%) of interpolation 720.00g, dry column-packing after mixing gets the post aspect ratio and is 20: 1 the dried post of silica gel; The tea-polyphenol 36.00g dry method that step (3) is obtained is splined on the dried post of silica gel, the mass ratio of tea-polyphenol and silica gel based filler is 1/200, under normal pressure, utilize pressure difference, take dehydrated alcohol: acetone=9: 1 (V/V) is as the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of EGCG, EGC, ECG under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively EGCG, EGC, ECG scrapes from the dried post of silica gel, add 95% ethanol, in ultrasonic wash-out 5 minutes, repeat wash-out 4 times, elutriant evaporated under reduced pressure with obtaining obtains respectively trimethyl-xanthine EGCG17.90g, EGC5.11g, ECG2.57g.
Embodiment 6
(1) except the foreign protein step: get the tea grounds 400g that is discarded in the Tea Production process, add water 2000ml, add the volume of water and the mass ratio of tea grounds is 5: 1 (V/W), after extracting 2 times under 90 ℃, filter behind the united extraction liquid, get filtrate 2800ml, the Tricholroacetic Acid aqueous solution that in filtrate, adds 186.67ml3%, adding the Tricholroacetic Acid aqueous solution is 1: 15 (V/V) with the filtrate volume ratio, and 8 ℃ left standstill 12 hours, obtains tea grounds Deproteinization extracting solution 2920ml after the centrifugal removal precipitation.
(2) polysaccharide precipitation step: the tea grounds Deproteinization extracting solution 2920ml that step (1) is obtained, add 584ml0.05g/ml cetyl pyridinium (CP-OH) aqueous solution, wherein, the volume ratio of polysaccharide precipitation agent and tea grounds Deproteinization extracting solution is 0.2: 1 (V/V), adjust pH6.0, react after 4 hours centrifugal being precipitated, with after dehydrated alcohol, acetone, the ether agitator treating precipitation, drying obtains tea polysaccharide 14.30g to precipitation successively.The supernatant liquor of centrifugal gained is evaporated to driedly, obtains tea grounds and removes polyoses extract 122.35g;
(3) the dried post separating step of the silica gel first time: the III level activated silica gel of getting 9298.60g, particle diameter 80 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 5%) of interpolation 489.40g, dry column-packing after mixing gets the post aspect ratio and is 10: 1 the dried post of silica gel; The tea grounds that step (2) is obtained goes polyoses extract 122.35g dry method to be splined on the dried post of silica gel, it is 1/80 that tea grounds removes the mass ratio of polyoses extract and silica gel based filler, under normal pressure, utilize pressure difference, methyl alcohol: ethyl acetate=1: 1 (V/V) is the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of trimethyl-xanthine and tea-polyphenol under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively trimethyl-xanthine and tea-polyphenol scrapes, add 95% ethanol from the dried post of silica gel, in ultrasonic wash-out 10 minutes, repeat wash-out 3 times, with the elutriant evaporated under reduced pressure that obtains, obtain respectively trimethyl-xanthine 13.90g and tea-polyphenol 41.75g
(4) the dried post separating step of the silica gel second time: the III level activated silica gel of getting 1983.12g, particle diameter 80 μ m, and the diatomite (mass percent of diatomite and silica gel based filler is 5%) of interpolation 104.38g, dry column-packing after mixing gets the post aspect ratio and is 10: 1 the dried post of silica gel; The tea-polyphenol 41.75g dry method that step (3) is obtained is splined on the dried post of silica gel, the mass ratio of tea-polyphenol and silica gel based filler is 1/50, utilizes pressure difference under normal pressure, and take dehydrated alcohol: acetone=8: 1 (V/V) is as the developping agent descending development, until solvent is opened up at the bottom of the post, stop the exhibition layer.
The silica gel thin-layer experiment obtains respectively the R of EGCG, EGC, ECG under same developping agent condition
fValue is according to the R that obtains
fAfter the silica gel based filler that value will be rich in respectively EGCG, EGC, ECG scrapes from the dried post of silica gel, add 95% ethanol, in ultrasonic wash-out 10 minutes, repeat wash-out 3 times, elutriant evaporated under reduced pressure with obtaining obtains respectively trimethyl-xanthine EGCG19.86g, EGC5.79g, ECG3.05g.
Claims (6)
1. the method for the standby various active material of interlock system from tea grounds comprises:
(1) except the foreign protein step; Get the tea grounds of being discarded in the Tea Production process, 70～100 ℃ of water extraction 2～4 times, add the volume of water and the mass ratio of tea grounds is 5: 1～15: 1 (V/W), filter behind the united extraction liquid, filtrate adds protein precipitant, foreign protein is removed in precipitin reaction, obtains tea grounds Deproteinization extracting solution after the centrifugal removal precipitation;
(2) polysaccharide precipitation step; Tea grounds Deproteinization extracting solution with step (1) obtains adds the polysaccharide precipitation agent, adjusts pH6.0～9.0, react after 4～12 hours, with after dehydrated alcohol, acetone, the ether agitator treating precipitation, drying obtains tea polysaccharide successively for centrifugal being precipitated respectively and supernatant liquor, gained precipitation; The supernatant liquor of gained is evaporated to driedly, obtains tea grounds and removes polyoses extract;
(3) the dried post separating step of the silica gel first time; The tea grounds that step (2) is obtained removes polyoses extract, be splined on the dried post of silica gel, it is 1/80～1/300 that tea grounds removes the mass ratio of polyoses extract and silica gel based filler, utilizes pressure difference with the developping agent descending development under normal pressure, obtains respectively trimethyl-xanthine and tea-polyphenol; Developping agent is the mixed solution of methyl alcohol and normal hexane or the mixed solution of methyl alcohol and ethyl acetate;
(4) the dried post separating step of the silica gel second time; The tea-polyphenol that step (3) is obtained, be splined on the dried post of silica gel, the mass ratio of tea-polyphenol and silica gel based filler is 1/50～1/200, under normal pressure, utilize pressure difference with the developping agent descending development, obtain respectively purity greater than 95% NVP-XAA 723 (EGCG), epigallocatechin (EGC), L-Epicatechin gallate (ECG); Developping agent is the mixed solution of dehydrated alcohol and normal hexane or the mixed solution of dehydrated alcohol and acetone.
As claimed in claim 1 a kind of from tea grounds the method for the standby various active material of interlock system, it is characterized in that: described except in the foreign protein step, described protein precipitant is: Freon 113 or 2～5% the Tricholroacetic Acid aqueous solution (V/V); Foreign protein is removed in described precipitin reaction, its process is: add Freon 113 in filtrate, adding Freon 113 is 1: 2～2: 1 (V/V) with the filtrate volume ratio, stirring reaction 10～20min, after the centrifugal removal precipitation, the water intaking layer obtains tea grounds Deproteinization extracting solution liquid; Or in filtrate, drip 2～5% the Tricholroacetic Acid aqueous solution, and adding the Tricholroacetic Acid aqueous solution is 1: 10～1: 20 (V/V) with the filtrate volume ratio, 5～10 ℃ left standstill 8～16 hours, obtained tea grounds Deproteinization extracting solution after the centrifugal removal precipitation.
As claimed in claim 1 a kind of from tea grounds the method for the standby various active material of interlock system, it is characterized in that: in the described polysaccharide precipitation step, described polysaccharide precipitation agent is: a kind of in 0.05g/ml cetyltrimethylammonium hydroxide Trimethylamine 99 bromide (CTA-OH) aqueous solution, 0.05g/ml cetyl pyridinium (CP-OH) aqueous solution, the volume ratio of polysaccharide precipitation agent and tea grounds Deproteinization extracting solution is 0.05: 1～0.2: 1 (V/V).
As claimed in claim 1 a kind of from tea grounds the method for the standby various active material of interlock system, it is characterized in that: in the dried post separating step of the described silica gel first time and the dried post separating step of silica gel for the second time:
The dried post of described silica gel is for to be filled with silica gel based filler, 5: 1～20: 1 separation column devices of aspect ratio, and the silica gel based filler is comprised of silica gel and diatomite, and the mass percent of diatomite and silica gel based filler is 5%～20%; The silica gel particle diameter is 30 μ m～80 μ m, and the silica gel activity is II～III level; The process of dry column-packing that the filling process of the dried post of described silica gel and general post separate employing is consistent.
As claimed in claim 1 a kind of from tea grounds the method for the standby various active material of interlock system, it is characterized in that: in the dried post separating step of the described silica gel first time:
The volume ratio of described developping agent is: methyl alcohol: normal hexane=1: 2～5: 1 (V/V), perhaps methyl alcohol: ethyl acetate=1: 3～4: 1 (V/V);
The process of described descending development is: after the loading, developping agent is added from the dried capital of silica gel, utilize the pressure difference descending development under normal pressure, when developer flow to silica gel is done the column bottom, stop the exhibition layer; After the silica gel based filler that is rich in respectively trimethyl-xanthine and tea-polyphenol scraped from the dried post of silica gel, add 95% ethanol, vibration wash-out 10～20 minutes or ultrasonic wash-out are 5～15 minutes on shaking table, repeat wash-out 2～4 times, with the elutriant evaporated under reduced pressure that obtains, namely obtain respectively trimethyl-xanthine and tea-polyphenol; The described silica gel based filler that is rich in respectively trimethyl-xanthine and tea-polyphenol, its residing position in the dried post of silica gel are the target product Rf value R that obtains with reference to silica gel thin-layer experiment under the identical developping agent condition
fDetermine.
As claimed in claim 1 a kind of from tea grounds the method for the standby various active material of interlock system, it is characterized in that: in the dried post separating step of the described silica gel second time:
The volume ratio of described developping agent is: dehydrated alcohol: normal hexane=8: 1～95: 5 (V/V), perhaps dehydrated alcohol: acetone=7: 1～9: 1 (V/V);
The process of described descending development is: after the loading, developping agent is added from the dried capital of silica gel, utilize the pressure difference descending development under normal pressure, when developer flow to silica gel is done the column bottom, stop the exhibition layer; After the silica gel based filler that is rich in respectively EGCG, EGC, ECG scraped from the dried post of silica gel, add 95% ethanol, vibration wash-out 10～20 minutes or ultrasonic wash-out are 5～15 minutes on shaking table, repeat wash-out 2～4 times, with the elutriant evaporated under reduced pressure that obtains, namely distinguish
Obtain purity greater than 95% EGCG, EGC, ECG; The described silica gel based filler that is rich in respectively EGCG, EGC, ECG, its residing position in the dried post of silica gel are the target product Rf value R that obtains with reference to silica gel thin-layer experiment under the identical developping agent condition
fDetermine.
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