CN102040610A - Novel method for simultaneously extracting caffeine, tea polyphenol and tea polysaccharide from tea using mechanochemical principle - Google Patents
Novel method for simultaneously extracting caffeine, tea polyphenol and tea polysaccharide from tea using mechanochemical principle Download PDFInfo
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Abstract
A novel method for simultaneously extracting caffeine, tea polyphenol and tea polysaccharide from tea using mechanochemical principles comprises the following steps: firstly, mixing tea raw materials and solid reagents in a mass ratio of 1:0.01-20, fully pulverizing the mixture for 1 min-60 min, taking out the pulverized powder, soaking the pulverized powder under stirring 1-10 times for 1-60 min with an organic solvent in an amount of 1-20 times the mass of the tea raw materials, filtering, collecting organic phase eluted a plurality of times, concentrating to obtain a mixture of caffeine and chlorophyll which is used to prepare caffeine by a regular method; secondly, soaking the solid tea powder in which caffeine and the chlorophyll have been removed with water in an amount of 1-5 times the mass of tea, adding acids to adjust the pH value to be not more than 7, soaking the pulverized powder under stirring 1-10 times for 1-60 min with a 1 to 20-fold amount of an organic solvent, filtering, collecting the tea polyphenol-containing organic solvent phase during each filtration, drying to obtain tea polyphenol, and if necessary, further purifying the tea polyphenol by other methods; thirdly, adding the tea residue processed in above steps into water in an amount of 5-10 times the volume of the tea residue, extracting at a temperature of 100 DEG C, centrifuging the extract to obtain a supernatant, adding anhydrous ethanol in an amount of 3 times the volume of the supernatant, allowing tea polysaccharide to precipitate for 24 h, centrifuging, and drying the precipitate to obtain the tea polysaccharide.
Description
(1) technical field
The present invention relates to a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously.
(2) technical background
Tea-polyphenol is the general name of polyhydroxy phenol analog derivative in the tealeaves, accounts for 15%～35% of dry weight of tea leaves; Its chemical constitution catechin accounts for 70% of tea-polyphenol total amount, also has flavones and flavonols, leucoanthocyanidin and anthocyanidin, phenolic acids and depside etc. in addition.Tea-polyphenol is a class ideal natural antioxidants, has a series of pharmacological functions such as anticancer, anti-ageing, radioprotective, removing human free radical, lowering blood glucose blood fat, is widely used in fields such as food-processing, medicines and health protection, daily-use chemical industries.
Also contain other functional component in addition in the tealeaves, caffeine has multiple physiologically active, accounts for the 1-5% of dry weight of tea leaves, and natural caffeine has huge demand in medical material market.The natural high moleculer eompound that tea polysaccharide is made up of hexose and five-carbon sugar accounts for the 1-2% of dry weight of tea leaves.The tea polysaccharide molecular-weight average is about 4 * 10
4Dalton, tea polysaccharide also comprises the small molecules oligose.That tea polysaccharide has is hypoglycemic, reducing blood-fat, strengthening immunity, atherosclerosis, anticoagulation, antithrombotic effect.
In the disclosed processing method of from tealeaves, extracting caffeine, tea-polyphenol and tea polysaccharide in the past, mainly can be divided into two stages: the fs: i.e. leaching stages.Method is: under heating condition (70-100 ℃), use a large amount of (general 14-20 times of tea quality) water or water and alcoholic acid mixed solution gradation (general 1-3 time) to carry out long-time (general 30min-60min) lixiviate, filter, concentrate the mixture water extract that obtains containing complicated components such as chlorophyll, caffeine, tea-polyphenol, tea polysaccharide, water-soluble protein, amino acid.As seen, have complex steps inevitably in conventional leaching stages, the production cycle is long, production cost is high, the drawback of lixiviate product component complexity.Also because water can dissolve part oxygen, can cause tea-polyphenol oxidation aggravation under heating condition simultaneously, the tea-polyphenol yield reduces.Subordinate phase: i.e. separation and purification stage.Method is: after obtaining containing the mixture tealeaves vat liquor of complicated components such as chlorophyll, caffeine, tea-polyphenol, tea polysaccharide, water-soluble protein, amino acid, through concentrating, adopt organic solvent extractionprocess, precipitation by metallic ion method, resin adsorption method or CO
2Subsequent technique methods such as supercritical extraction are carried out separation and purification respectively to compositions such as the tea-polyphenol in the mixture, caffeine and tea polysaccharide respectively.As seen, conventional purification phase also need to adopt material, energy charge huge concentrate, finished product that purifying process just can be produced caffeine, tea-polyphenol, tea polysaccharide.Based on above reason, continue to seek efficient, consumption reduction, leach extraction method, and high efficiency caffeine cheaply, tea-polyphenol and tea polysaccharide separation purification method, be the improved emphasis direction of tea component extraction process.
Be to improve the tea component extracting technology, and patent application " a kind of method of from tealeaves, extracting tea-polyphenol and separating monomer EGCG (number of patent application: 200810059567.0) " first the mechanochemistry principle is applied in the extraction of tea-polyphenol.Its method is: with tealeaves and solid alkali reagent mixing, the common grinding, with water dissolution, stirring, centrifugal, get supernatant liquor, add mineral acid and regulate supernatant liquor pH≤8.0, produce and precipitate, filter monomer EGCG.Gained concentrating filter liquor, the dry crude product tea-polyphenol that gets.This method has that step is simple, easy to operate, the advantage of constant product quality.In addition, the advantage that this patent is the most outstanding is: do not need heating at the tea-polyphenol leaching process, therefore can to a certain degree reduce production costs; And, therefore can avoid the tea-polyphenol oxidation, and then tea-polyphenol yield and purity are improved because the tea-polyphenol leaching process need not heat.The method of this patent disclosure has been opened up the new field of tea component leach extraction method.
Though the disclosed method of this patent application has certain improvement than conventional tea polyphenol leach extraction method, but this method fails to give full play to the unique advantage that mechanochemical reaction extracts tea-polyphenol, there is many-sided improved place that is worth: the first, adopt this method gained tea-polyphenol purity lower (≤77%), contain a large amount of impurity, as: a large amount of metal-salts, caffeine, tea polysaccharide, protein etc., must pass through a large amount of follow-up complicated technologies, as: organic solvent extractionprocess, precipitation by metallic ion method, resin adsorption method, CO
2Supercritical extractions etc. continue purifying to gained low-purity tea-polyphenol.The directed advantage of extracting tea-polyphenol of mechanochemical reaction can't embody; The second, tea-polyphenol easy deterioration by oxidation under alkaline condition, this patent application directly uses alkali solid reagent and tealeaves to carry out common grinding, can cause tea-polyphenol oxidation aggravation, and this is a lower major reason of tea-polyphenol yield that causes by this method production; Three, directly use water extraction tea-polyphenol metal-salt in the open method of this patent application, and reckon without the influence factor of other restriction tea-polyphenol or the strippings of tea-polyphenol metal-salt, this directly causes adopting this method to extract tea-polyphenol inefficiency, the average yield of tea-polyphenol≤17%; Four, the open method of this patent application recommends directly to go out tea-polyphenol or tea-polyphenol metal-salt with 20 times of volumes of tea quality are water-soluble, and this can cause in follow-up concentrate drying process energy charge huge, and facility investment costliness, the purpose that reduces production costs are difficult to realization; Five, this patent application recommends to use alkali, strong base-weak acid salt or the neutral salt of a large amount of sodium (Na), copper (Cu), aluminium (Al), calcium metal ions such as (Ca) as solid reaction reagent, and this patent does not provide desalination method, tea-polyphenol metal (or the heavy metal that this can cause this method to be produced, as: copper (Cu)) salt residual quantity is too high, has seriously limited the utilization scope of the tea-polyphenol product that adopts this method production; Six, the solid waste that adopts this method to produce contains the metal-salt (metal-salt content 〉=10%) of high density, unprocessedly can not directly transform into agricultural fertilizer and animal-feed, can cause serious environmental to be polluted.
For overcome patent application " a kind of method of from tealeaves, extracting tea-polyphenol and separating monomer EGCG; (and number of patent application: 200810059567.0) " defective, give full play to the advantage of mechanochemistry aspect the extraction tea-polyphenol, the particularly directed advantage of extracting tea-polyphenol the invention discloses a kind of novel method of utilizing the mechanochemistry principle to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously from tealeaves
The present invention is based on the mechanochemistry ratio juris, adopt following invention thinking: the first step, tea-polyphenol are the polyhydroxy phenol compounds, are slightly acidic, can with the effect of alkali solid reaction reagent, generate tea-polyphenol salt soluble in water.This moment, tea-polyphenol salt polarity increased, and the solubleness in organic solvent declines to a great extent.When wash-out with an organic solvent during through tealeaves that mechanochemical reaction is handled, tea-polyphenol salt is insoluble to organic solvent, therefore not by wash-out; And other impurity such as caffeine, chlorophyll etc. still are in unbound state, can and be present in the organic phase by wash-out, can realize that by this step the tea-polyphenol product removes chlorophyll, caffeine and other polarity purpose than small impurities, the caffeine in the organic phase can obtain purifying by ordinary method; Second step: when with caffeine, after chlorophyll is removed, directly in tea-leaf power, add mineral acid and tea-polyphenol reactant salt generation free tea-polyphenol again, this moment, tea-polyphenol polarity reduced, solubleness in organic solvent is improved, when using the organic solvent wash-out once more, can be by the smooth stripping of organic solvent, realize the purpose that tea-polyphenol extracts, when with an organic solvent extracting tea-polyphenol, also can be by the kind and the proportioning of control organic solvent, and then water soluble tea polysaccharide in the control tealeaves, protein, metal-salt and other polarity is the stripping of impurity greatly, realizes the purpose of tea-polyphenol purifying synchronously; The 3rd step: after realizing the separating one by one of caffeine, chlorophyll and tea-polyphenol, tea leaf residual can use the hot water lixiviate, the employing ordinary method prepares tea polysaccharide.
Disclosed by the invention a kind of utilize the mechanochemistry principle extracts caffeine, tea-polyphenol and tea polysaccharide simultaneously from tealeaves novel method and patent application " a kind of method of from tealeaves, extracting tea-polyphenol and separating monomer EGCG; (and number of patent application: 200810059567.0) " though all adopt the mechanochemistry ultimate principle, invention thinking and production technique exist fundamental difference.In addition this patent and patent application " a kind of method of from tealeaves, extracting tea-polyphenol and separating monomer EGCG; (number of patent application: 200810059567.0) " disclosed method or in the past common process compare and exist huge advantage, be mainly reflected in the following aspects: first, the present invention gives full play to the advantage of mechanochemical reaction in orientation extraction tea-polyphenol, realized limit purifying in the tea-polyphenol leaching process, the purpose that extract on the limit, caffeine in the gained tea-polyphenol, tea polysaccharide, protein, inorganic salt content declines to a great extent, and need not to adopt organic solvent extractionprocess, the precipitation by metallic ion method, resin adsorption method or CO
2Under the situation of subsequent purification methods such as supercritical extraction, purity is significantly improved, and tea-polyphenol purity 〉=90% directly can be used as high-grade tea-polyphenol product and sells; The second, the present invention has taken into full account the influence factor of restriction tea-polyphenol leaching yield and has caused tea-polyphenol oxidized influence factor in leaching process, and the tea-polyphenol yield significantly improves, tea-polyphenol yield 〉=20%; Three, the present invention uses protection reagent potassium borate first, can alleviate the oxidation in the common process of lapping of tealeaves and alkaline reagents, improves the tea-polyphenol yield; Four, the present invention uses the strong base-weak acid salt of potassium hydroxide, saleratus, salt of wormwood, potassium silicate, potassium primary phosphate, dipotassium hydrogen phosphate, Repone K or other potassium as solid reaction reagent first, recommend to use phosphoric acid to regulate with acid as the pH value, main inorganic salt are potassiumphosphate, potassium hydrogen phosphate, potassium primary phosphate in the solid waste of tea-polyphenol extraction back, therefore the solid waste that adopts method disclosed by the invention to produce can directly be used no noxious waste pollution in agricultural as potassium, phosphate fertilizer.Five, the present invention has realized the purpose that extract on each composition limit purifying, limit because of the introducing of mechanochemistry principle, can realize the purifying of caffeine, tea-polyphenol, tea polysaccharide one by one, and tea resources is fully used.Six, the present invention has significantly reduced the usage quantity of water, has avoided concentration process required a large amount of energy wastees and facility investment.
To sum up, a kind of novel method of utilizing the mechanochemistry principle to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously from tealeaves disclosed by the invention has realized raising tea-polyphenol yield, raising tea-polyphenol purity, the purposes such as step, shortening production cycle, constant product quality, no noxious waste pollution of simplifying.Tea resources is fully used simultaneously, not only can obtain highly purified tea-polyphenol, can also extract simultaneously and obtain caffeine, tea polysaccharide.The waste of production process also can be used as chemical fertilizer or feed obtains utilizing in agricultural, and present method greatly reduces production cost, has improved overall economic efficiency.By literature search, yet there are no the report of similar approach.
(3) summary of the invention
Mentality of designing of the present invention is: the first step, tea-polyphenol are the polyhydroxy phenol compounds, are slightly acidic, can with the effect of alkali solid reaction reagent, generate tea-polyphenol salt soluble in water.This moment, tea-polyphenol salt polarity increased, and the solubleness in organic solvent declines to a great extent.When wash-out with an organic solvent during through tealeaves that mechanochemical reaction is handled, tea-polyphenol salt is insoluble to organic solvent, therefore not by wash-out; And other impurity such as caffeine, chlorophyll etc. still are in unbound state, can and be present in the organic phase by wash-out, can realize that by this step the tea-polyphenol product removes chlorophyll, caffeine and other polarity purpose than small impurities, the caffeine in the organic phase can obtain purifying by ordinary method; Second step: after caffeine, chlorophyll are removed, directly in tea-leaf power, add mineral acid and tea-polyphenol reactant salt generation free tea-polyphenol again, this moment, tea-polyphenol polarity reduced, solubleness in organic solvent is improved, when using the organic solvent wash-out once more, can be realized the purpose that tea-polyphenol extracts by the smooth stripping of organic solvent.When with an organic solvent extracting tea-polyphenol, also can pass through the kind and the proportioning of control organic solvent, and then water soluble tea polysaccharide, protein, metal-salt and other polarity realize the purpose of tea-polyphenol purifying synchronously than the stripping of big impurity in the control tealeaves; The 3rd step: after realizing the separating one by one of caffeine, chlorophyll and tea-polyphenol, tea leaf residual can use the hot water lixiviate, the employing ordinary method prepares tea polysaccharide.
The technical solution used in the present invention is specific as follows:
A kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously: the first step, tea raw material and solid-phase reagent mass ratio 1: 0.01-20 are mixed, mixture is fully ground 1min-60min, take out abrasive flour, with 1-20 times of organic solvent of tea raw material quality, divide and soak and stir 1min-60min respectively 1-10 time, filter, collect repeatedly wash-out organic phase, concentrate, get caffeine and chlorophyllous mixture, this mixture adopts ordinary method to prepare caffeine; Second the step, will remove caffeine and chlorophyllous solid tea-leaf power, add 1-5 times of water infiltration of tea quality, add acid for adjusting pH value≤7, with 1-20 times of organic solvent, divide and soak and stir 1min-60min respectively 1-10 time, filter, collect each time and contain the organic solvent phase of tea-polyphenol, the dry tea-polyphenol that gets, if needed, tea-polyphenol can also be further purified by additive method; The 3rd step: the tea leaf residual that will handle through above-mentioned steps, adds 5-10 times of volume water, 100 ℃ of lixiviates, the centrifuging and taking supernatant liquor adds 3 times of these supernatant liquor volume dehydrated alcohols precipitation tea polysaccharide 24h, and is centrifugal, get and precipitate drying acquisition tea polysaccharide.
Solid-phase reagent of the present invention comprises solid state reaction reagent and protective material, and solid state reaction reagent and protective material mass ratio are 1: 0.01-1.
Solid state reaction reagent of the present invention can be selected from following one or both and reach above arbitrary combination: potassium hydroxide, saleratus, salt of wormwood, Potassium ethanoate, potassium silicate, potassium primary phosphate, dipotassium hydrogen phosphate, Repone K, or the strong base-weak acid salt of other potassium, also can use sodium hydroxide, aluminium hydroxide, calcium hydroxide, copper hydroxide, sodium bicarbonate, yellow soda ash, lime carbonate, water glass, SODIUM PHOSPHATE, MONOBASIC, sodium-chlor, magnesium chloride, S-WAT, aluminum chloride, alkali such as calcium chloride, strong base-weak acid salt, the present invention recommends preferred solid state reaction reagent to be selected from following one or both and reaches above arbitrary combination: potassium hydroxide, saleratus, salt of wormwood, Potassium ethanoate, potassium silicate, potassium primary phosphate, dipotassium hydrogen phosphate, Repone K, or the strong base-weak acid salt of other potassium.
Protective material of the present invention is that following one or both reach above arbitrary combination: boric acid, Sodium Tetraborate, potassium borate, lime borate or other borate, it is potassium borate that the present invention recommends preferred protective material.
Tea raw material of the present invention and solid-phase reagent mass ratio are 1: it is 1 that 0.01-20, the present invention recommend preferred tea raw material and solid-phase reagent mass ratio: 0.1-1.
The milling time of tea raw material of the present invention and solid-phase reagent is 1min-60min, and the present invention recommends more preferably that the time is 10-20min.
Wash-out caffeine and the chlorophyllous organic solvent of being used for of the present invention is selected from following one or both and above arbitrary combination: sherwood oil, hexane, hexanaphthene, octane-iso, trifluoroacetic acid, trimethylpentane, pentamethylene, heptane, Butyryl Chloride, trieline, tetracol phenixin, trichlorotrifluoroethane, propyl ether, toluene, p-Xylol, chlorobenzene, orthodichlorobenzene, ether, benzene, isopropylcarbinol, methylene dichloride, ethylene dichloride, propyl carbinol, N-BUTYL ACETATE, propyl alcohol, mibk, tetrahydrofuran (THF), ethyl acetate, Virahol, chloroform, methyl ethyl ketone, dioxan, pyridine, acetone, Nitromethane 99Min., ethanol, acetate, acetonitrile, aniline, dimethyl formamide, methyl alcohol, ethylene glycol, methyl-sulphoxide.The present invention recommends preferred organic solvent to be selected from following one or both and reaches above arbitrary combination: sherwood oil, hexanaphthene, ether, ethyl acetate, ethanol.
Of the present inventionly be used for the wash-out caffeine and chlorophyllous consumption of organic solvent is that tea quality 1-20 doubly divides wash-out 1-10 time, the more preferably consumption of organic solvent that the present invention recommends be 4-10 doubly, the preferred wash-out number of times that the present invention recommends is 2-5 time.
Organic solvent wash-out caffeine of the present invention and chlorophyllous each soak time are 1min-60min, and the preferred stirring soak time that the present invention recommends is 5-15min.
Of the present invention from caffeine and chlorophyll mixture the employing ordinary method of preparation caffeine can be selected from the combination of following one or both and above method: liquid-liquid extraction, Solid-Phase Extraction, subliming method, CO
2Supercritical extraction, the preferred preparation method that the present invention recommends is a subliming method.
The of the present invention extraction the tealeaves pressed powder behind decaffeination, chlorophyll in the tea-polyphenol process need add less water and soak into, amount of water be tea quality 1-5 doubly, the present invention recommend preferred amount of water be tea quality 1-3 doubly.
Of the present invention the tealeaves pressed powder behind decaffeination, chlorophyll, the extraction in the tea-polyphenol process, need in the tea-leaf power of water infiltration, add acid for adjusting pH value, and make pH≤7, the used acid of adjusting pH value can be selected from following one or both and reach above arbitrary combination: sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, citric acid, it is phosphoric acid that the present invention recommends preferred acid.
Of the present invention from decaffeination, extract in the tea-polyphenol process in the tealeaves pressed powder behind the chlorophyll, after adding water infiltration and adding acid for adjusting pH value, need to add the organic solvent extraction tea-polyphenol, the organic solvent that extracts tea-polyphenol can be selected from following one or both and reach above arbitrary combination: sherwood oil, hexane, hexanaphthene, octane-iso, trifluoroacetic acid, trimethylpentane, pentamethylene, heptane, Butyryl Chloride, trieline, tetracol phenixin, trichlorotrifluoroethane, propyl ether, toluene, p-Xylol, chlorobenzene, orthodichlorobenzene, ether, benzene, isopropylcarbinol, methylene dichloride, ethylene dichloride, propyl carbinol, N-BUTYL ACETATE, propyl alcohol, mibk, tetrahydrofuran (THF), ethyl acetate, Virahol, chloroform, methyl ethyl ketone, dioxan, pyridine, acetone, Nitromethane 99Min., ethanol, acetate, acetonitrile, aniline, dimethyl formamide, methyl alcohol, ethylene glycol, methyl-sulphoxide, the present invention recommends preferred organic solvent to be selected from following one or both and above arbitrary combination: propyl carbinol, ether, ethyl acetate, acetone, ethanol, methyl alcohol.
Of the present invention the tealeaves pressed powder behind decaffeination, chlorophyll, the extraction in the tea-polyphenol process, after adding water infiltration and adding acid for adjusting pH value, need to add the organic solvent soaking and stirring, the organic solvent quality that is used to stir immersion be tea quality 1-20 doubly, divide 1-10 soaking and stirring, it is 6-12 times that the present invention recommends preferred consumption of organic solvent, and preferred soaking and stirring number of times is 3-6 time.
Of the present invention the tealeaves pressed powder behind decaffeination, chlorophyll, the extraction in the tea-polyphenol process, need to add the organic solvent soaking and stirring, each soaking and stirring time is 1min-60min, and it is 5-10min that the present invention recommends the preferred soaking and stirring time.
Product tea-polyphenol of the present invention is further purified method can be selected from following one or both methods and above arbitrary combination: liquid-liquid extraction method, precipitation by metallic ion method, solid phase extraction or CO
2Supercritical extraction.
Of the present invention the tealeaves pressed powder after having extracted caffeine, chlorophyll and tea-polyphenol, the extraction in the tea polysaccharide process, need add 5-10 times of water again, 100 ℃ of lixiviates, the centrifuging and taking supernatant liquor, add 3 times of these supernatant liquor volume dehydrated alcohols precipitation tea polysaccharide 24h, centrifugal, get the dry tea polysaccharide that obtains of precipitation.
The concrete described extracting method of the present invention carries out according to following steps: the first step, tea raw material and solid-phase reagent mass ratio 1: 0.01-20 are mixed, mixture is fully ground 1min-60min, take out abrasive flour, with 1-20 times of organic solvent of tea raw material quality, divide and soak and stir 1min-60min respectively 1-10 time, filter, collect repeatedly wash-out organic phase, concentrate, get caffeine and chlorophyllous mixture, this mixture adopts ordinary method to prepare caffeine; Second the step, will remove caffeine and chlorophyllous solid tea-leaf power, add 1-5 times of water infiltration of tea quality, add acid for adjusting pH value≤7, with 1-20 times of organic solvent, divide and soak and stir 1min-60min respectively 1-10 time, filter, collect each time and contain the organic solvent phase of tea-polyphenol, the dry tea-polyphenol that gets, if needed, tea-polyphenol can also be further purified by additive method; The 3rd step: the tea leaf residual that will handle through above-mentioned steps, adds 5-10 times of volume water, 100 ℃ of lixiviates, the centrifuging and taking supernatant liquor adds 3 times of these supernatant liquor volume dehydrated alcohols precipitation tea polysaccharide 24h, and is centrifugal, get and precipitate drying acquisition tea polysaccharide.
Beneficial effect of the present invention:
(1) the present invention gives full play to the advantage of mechanochemical reaction in orientation extraction tea-polyphenol, realized the purpose that extract on limit purifying in the tea-polyphenol leaching process, limit, make that caffeine, tea polysaccharide, protein, inorganic salt content decline to a great extent in the gained tea-polyphenol, purity is significantly improved, tea-polyphenol purity 〉=90%.Can be directly sell as high quality tea-polyphenol product, need not subsequent purification technology, as solid phase extraction, liquid-liquid extraction method, precipitation by metallic ion method, CO
2Supercritical extraction etc.
(2) the present invention has taken into full account and has adopted the mechanochemistry principle to prepare the influence factor of restriction tea-polyphenol leaching yield in the tea-polyphenol technology and cause tea-polyphenol oxidized influence factor in leaching process, and the tea-polyphenol yield significantly improves, tea-polyphenol yield 〉=20%.
(3) the present invention uses the strong base-weak acid salt of potassium hydroxide, saleratus, salt of wormwood, Potassium ethanoate, potassium silicate, potassium primary phosphate, dipotassium hydrogen phosphate, Repone K or other potassium as solid reaction reagent first, recommend to use phosphoric acid to regulate with acid as the pH value, main inorganic salt are potassiumphosphate, potassium hydrogen phosphate, potassium primary phosphate in the solid waste of tea-polyphenol extraction back, therefore the solid waste that adopts production method disclosed by the invention to produce can directly be used no noxious waste pollution in agricultural as potassium, phosphate fertilizer.
(4) the present invention uses protection reagent potassium borate first, can alleviate the oxidation in the common process of lapping of tealeaves and alkaline reagents, improves the tea-polyphenol yield.
(5) the present invention has significantly reduced the use of water, has avoided technology required a large amount of energy wastees and facility investment of concentration process in producing the tea-polyphenol process in the past.
(6) the present invention fully takes into account the comprehensive utilization of tealeaves, adopts the method for substep purifying, extraction, realizes the extraction of caffeine, tea-polyphenol, tea polysaccharide one by one, makes tea resources obtain comprehensive utilization.
(7) the open tea-polyphenol extracting method of the present invention has been realized improving the tea-polyphenol yield, has improved tea-polyphenol purity, has simplified step, has been shortened the production cycle, the purpose that significantly reduces production costs has been fully used, has been realized to constant product quality, no noxious waste pollution, tea resources.
Description of drawings
Accompanying drawing is a kind of novel method schematic flow sheet that utilizes the mechanochemistry principle to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously from tealeaves
(4) embodiment
Below with concrete practical work example technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto.
The qualitative and quantitative analysis method of product:
The tea-polyphenol total content is measured in the product: adopt the GB/T-83132002 standard.
Content of caffeine is measured in the product tea-polyphenol: adopt the GB/T-83132008 standard.
Tea polysaccharide assay: anthrone-sulfuric acid process
Embodiment 1
Under the room temperature, 10g broken tea raw material is mixed with 1g salt of wormwood, 0.2g Sodium Tetraborate, with mixture in grinding in ball grinder 10min; Take out abrasive flour, divide to add the 20mL chloroform respectively 3 times in the mixing tea-leaf power, stir 10min at every turn, filter, merge 3 times and handle gained chloroform phase, concentrate, get chlorophyll and caffeine mixture, this mixture adopts subliming method to produce caffeine; Adding 20mL water and 2mL phosphoric acid in chloroform wash-out gained tealeaves solid are regulated pH value≤7, divide to add ethyl acetate 20mL wash-out tealeaves solid once more for 5 times respectively, stir 10min, filter, and collect ethyl acetate phase elutriant 5 times, concentrate, and get tea-polyphenol; The tealeaves solid that disposes through above-mentioned steps adds 100mL water, is heated to 100 ℃ and be incubated 20min, filters, and adds 300mL ethanol, leaves standstill 24h, the tea polysaccharide of collecting precipitation, exsiccant tea polysaccharide.Get caffeine 0.131g through above-mentioned steps, purity 99%; Get tea-polyphenol 2.3g, purity 95%; Get tea polysaccharide 0.21g, purity 50%.
Embodiment 2
Under the room temperature, 10g broken tea raw material is mixed with 1.2g potassium silicate, 0.2g Sodium Tetraborate, with mixture in grinding in ball grinder 10min; Take out abrasive flour, in mixing tea-leaf power, divide and add 20mL petroleum ether-ethyl acetate (volume ratio 1: 1) mixing solutions respectively 5 times, stir 10min respectively, filter, merge five times and handle gained petroleum ether-ethyl acetate phase, concentrate, get chlorophyll and caffeine mixture, this mixture adopts subliming method to produce caffeine; Adding 10mL water and 2mL phosphoric acid in petroleum ether-ethyl acetate wash-out gained tealeaves solid are regulated pH value≤7, divide to add dehydrated alcohol 20mL wash-out tealeaves solid once more for 5 times respectively, stir 10min, filter, and collect 5 ethanol moving phases and concentrate, and get tea-polyphenol; The tealeaves solid that disposes through above-mentioned steps adds 100mL water, is heated to 100 ℃ and be incubated 20min, filters, and adds 300mL ethanol, leaves standstill 24h, collecting precipitation dry tea polysaccharide.Get caffeine 0.128g through above-mentioned steps, purity 98.6%; Get tea-polyphenol 2.2g, purity 90.9%; Get tea polysaccharide 0.20g, purity 52%.
Embodiment 3
Under the room temperature, 10g broken tea raw material is mixed with 1g saleratus, 0.2g Sodium Tetraborate, with mixture in grinding in ball grinder 10min; Take out abrasive flour, in mixing tea-leaf power, divide and add 20mL sherwood oil-chloroform (volume ratio 1: 1) mixing solutions respectively 5 times, stir 10min respectively, filter, merge five times and handle gained sherwood oil-chloroform phase, concentrate, get chlorophyll and caffeine mixture, this mixture adopts subliming method to produce caffeine; Adding 10mL water and 2mL phosphoric acid in sherwood oil-chloroform wash-out gained tealeaves solid are regulated pH value≤7, divide to add dehydrated alcohol 20mL wash-out tealeaves solid once more for 5 times respectively, stir 10min, filter, and collect 5 ethanol moving phases and concentrate, and get tea-polyphenol; The tealeaves solid that disposes through above-mentioned steps adds 100mL water, is heated to 100 ℃ and be incubated 20min, filters, and adds 300mL ethanol, leaves standstill 24h, collecting precipitation dry tea polysaccharide.Get caffeine 0.129g through above-mentioned steps, purity 99%; Get tea-polyphenol 2.15g, purity 91%; Get tea polysaccharide 0.21g, purity 51%.
Embodiment 4
Under the room temperature, 10g broken tea raw material is mixed with 1.2g salt of wormwood, 0.2g Sodium Tetraborate, with mixture in grinding in ball grinder 10min; Take out abrasive flour, divide to add the 20mL dehydrated alcohol respectively 5 times in the mixing tea-leaf power, stir 10min respectively, filter, merge five times and handle gained ethanol phase, concentrate, get chlorophyll and caffeine mixture, this mixture adopts subliming method to produce caffeine; Adding 10mL water and 2mL phosphoric acid in ethanol elution gained tealeaves solid are regulated pH value≤7, divide to add dehydrated alcohol 20mL wash-out tealeaves solid once more for 5 times respectively, stir 10min, filter, and collect 5 ethanol moving phases and concentrate, and get tea-polyphenol; The tealeaves solid that disposes through above-mentioned steps adds 100mL water, is heated to 100 ℃ and be incubated 20min, filters, and adds 300mL ethanol, leaves standstill 24h, collecting precipitation dry tea polysaccharide.Get caffeine 0.134g through above-mentioned steps, purity 99%; Get tea-polyphenol 1.8g, purity 91.5%; Get tea polysaccharide 0.22g, purity 53%.
Embodiment 5
Under the room temperature, 10g broken tea raw material is mixed with 1.2g saleratus, 0.2g Sodium Tetraborate; With mixture in grinding in ball grinder 10min; Take out abrasive flour, divide to add the 20mL ethyl acetate respectively 5 times in the mixing tea-leaf power, stir 10min respectively, filter, merge five times and handle gained ethyl acetate phase, concentrate, get chlorophyll and caffeine mixture, this mixture adopts subliming method to produce caffeine; Add 10mL water and 2mL phosphoric acid in eluent ethyl acetate gained tealeaves solid, regulate pH value≤7, divides to add ethyl acetate 20mL wash-out tealeaves solid once more for 5 times respectively, stir 10min, filter, it is mobile concentrated mutually to collect 5 ethyl acetate, gets tea-polyphenol; The tealeaves solid that disposes through above-mentioned steps adds 100mL water, is heated to 100 ℃ and be incubated 20min, filters, and adds 300mL ethanol, leaves standstill 24h, collecting precipitation dry tea polysaccharide.Get caffeine 0.114g through above-mentioned steps, purity 99%; Get tea-polyphenol 2.12g, purity 95%; Get tea polysaccharide 0.25g, purity 55%.
Embodiment 6
Under the room temperature, 10g broken tea raw material is mixed with 0.6g saleratus, 0.6g salt of wormwood and 0.2g Sodium Tetraborate; With mixture in grinding in ball grinder 10min; Take out abrasive flour, divide to add the 20mL ethyl acetate respectively 5 times in the mixing tea-leaf power, stir 10min respectively, filter, merge five times and handle gained ethyl acetate phase, concentrate, get chlorophyll and caffeine mixture, this mixture adopts subliming method to produce caffeine; Adding 10mL water and 2mL phosphoric acid in eluent ethyl acetate gained tealeaves solid are regulated pH value≤7, divide to add ethanol 20mL wash-out tealeaves solid once more for 5 times respectively, stir 10min, filter, and collect 5 ethanol moving phases and concentrate, and get tea-polyphenol; The tealeaves solid that disposes through above-mentioned steps adds 100mL water, is heated to 100 ℃ and be incubated 20min, filters, and adds 300mL ethanol, leaves standstill 24h, collecting precipitation dry tea polysaccharide.Get caffeine 0.122g through above-mentioned steps, purity 99%; Get tea-polyphenol 2.35g, purity 90.3%; Get tea polysaccharide 0.1.93g, purity 53%.
Embodiment 7
Under the room temperature, 10g broken tea raw material is mixed with 0.6g saleratus, 0.6g salt of wormwood and 0.2g Sodium Tetraborate; With mixture in grinding in ball grinder 10min; Take out abrasive flour, divide to add the 20mL ethyl acetate respectively 2 times in the mixing tea-leaf power, stir 10min respectively, filter, merge five times and handle gained ethyl acetate phase, concentrate, get chlorophyll and caffeine mixture, this mixture adopts subliming method to produce caffeine; Adding 10mL water and 2mL phosphoric acid in eluent ethyl acetate gained tealeaves solid are regulated pH value≤7, divide to add ethanol 20mL wash-out tealeaves solid once more for 5 times respectively, stir 10min, filter, and collect 5 ethanol moving phases and concentrate, and get tea-polyphenol; The tealeaves solid that disposes through above-mentioned steps adds 100mL water, is heated to 100 ℃ and be incubated 20min, filters, and adds 300mL ethanol, leaves standstill 24h, collecting precipitation dry tea polysaccharide.Get caffeine 0.9g through above-mentioned steps, purity 99%; Get tea-polyphenol 2.55g, purity 91.2%; Get tea polysaccharide 0.19g, purity 52.9%.
Embodiment 8
Under the room temperature, 10g broken tea raw material is mixed with 1.2g Potassium ethanoate and 0.2g Sodium Tetraborate; With mixture in grinding in ball grinder 10min; Take out abrasive flour, divide to add the 20mL ethyl acetate respectively 2 times in the mixing tea-leaf power, stir 10min respectively, filter, merge five times and handle gained ethyl acetate phase, concentrate, get chlorophyll and caffeine mixture, this mixture adopts subliming method to produce caffeine; Adding 30mL water and 2mL phosphoric acid in eluent ethyl acetate gained tealeaves solid are regulated pH value≤7, divide to add ethanol 20mL wash-out tealeaves solid once more for 5 times respectively, stir 10min, filter, and collect 5 ethanol moving phases and concentrate, and get tea-polyphenol; The tealeaves solid that disposes through above-mentioned steps adds 100mL water, is heated to 100 ℃ and be incubated 20min, filters, and adds 300mL ethanol, leaves standstill 24h, collecting precipitation dry tea polysaccharide.Get caffeine 0.9g through above-mentioned steps, purity 99%; Get tea-polyphenol 2.75g, purity 92.3%; Get tea polysaccharide 0.16g, purity 52.9%.
Claims (17)
1. novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously: the first step, tea raw material and solid-phase reagent mass ratio 1:0.01-20 are mixed, mixture is fully ground 1min-60min, take out abrasive flour, with 1-20 times of organic solvent of tea raw material quality, divide and soak and stir 1min-60min respectively 1-10 time, filter, collect repeatedly wash-out organic phase, concentrate, get caffeine and chlorophyllous mixture, this mixture adopts ordinary method to prepare caffeine; Second the step, will remove caffeine and chlorophyllous solid tea-leaf power, add 1-5 times of water infiltration of tea quality, add acid for adjusting pH value≤7, with 1-20 times of organic solvent, divide and soak and stir 1min-60min respectively 1-10 time, filter, collect each time and contain the organic solvent phase of tea-polyphenol, the dry tea-polyphenol that gets, if needed, tea-polyphenol can also be further purified by additive method; The 3rd step: the tea leaf residual that will handle through above-mentioned steps, adds 5-10 times of volume water, 100 ℃ of lixiviates, the centrifuging and taking supernatant liquor adds 3 times of these supernatant liquor volume dehydrated alcohols precipitation tea polysaccharide 24h, and is centrifugal, get and precipitate drying acquisition tea polysaccharide.
2. a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol, tea polysaccharide simultaneously as claimed in claim 1; it is characterized in that described solid-phase reagent comprises solid state reaction reagent and protective material, solid state reaction reagent and protective material mass ratio are 1: 0.01-1.
3. solid state reaction reagent as claimed in claim 2, it is characterized in that described solid state reaction reagent can be selected from following one or both and reach above arbitrary combination: potassium hydroxide, saleratus, salt of wormwood, Potassium ethanoate, potassium silicate, potassium primary phosphate, dipotassium hydrogen phosphate, Repone K, or other potassium ground strong base-weak acid salt, also can use sodium hydroxide, aluminium hydroxide, calcium hydroxide, copper hydroxide, sodium bicarbonate, yellow soda ash, lime carbonate, water glass, SODIUM PHOSPHATE, MONOBASIC, sodium-chlor, magnesium chloride, S-WAT, aluminum chloride, alkali such as calcium chloride, strong base-weak acid salt, the present invention recommends preferred solid state reaction reagent to be selected from following one or both and reaches above arbitrary combination: potassium hydroxide, saleratus, salt of wormwood, Potassium ethanoate, potassium silicate, potassium primary phosphate, dipotassium hydrogen phosphate, Repone K, or the strong base-weak acid salt of other potassium.
4. protective material as claimed in claim 2; it is characterized in that described described protective material is that following one or both reach above arbitrary combination: boric acid, Sodium Tetraborate, potassium borate, lime borate or other borate, it is potassium borate that the present invention recommends preferred protective material.
5. a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously as claimed in claim 1, it is characterized in that described tea raw material and solid-phase reagent mass ratio are 1: it is 1 that 0.01-20, the present invention recommend preferred tea raw material and solid-phase reagent mass ratio: 0.1-1.
6. a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously as claimed in claim 1, it is characterized in that described tea raw material and solid-phase reagent milling time are 1min-60min, the present invention recommends more preferably that the time is 10-20min.
7. a kind of mechanochemistry principle of utilizing as claimed in claim 1 is extracted caffeine simultaneously from tealeaves, the novel method of tea-polyphenol and tea polysaccharide is characterized in that described wash-out caffeine and the chlorophyllous organic solvent of being used for is selected from following one or both and above arbitrary combination: sherwood oil, hexane, hexanaphthene, octane-iso, trifluoroacetic acid, trimethylpentane, pentamethylene, heptane, Butyryl Chloride, trieline, tetracol phenixin, trichlorotrifluoroethane, propyl ether, toluene, p-Xylol, chlorobenzene, orthodichlorobenzene, ether, benzene, isopropylcarbinol, methylene dichloride, ethylene dichloride, propyl carbinol, N-BUTYL ACETATE, propyl alcohol, mibk, tetrahydrofuran (THF), ethyl acetate, Virahol, chloroform, methyl ethyl ketone, dioxan, pyridine, acetone, Nitromethane 99Min., ethanol, acetate, acetonitrile, aniline, dimethyl formamide, methyl alcohol, ethylene glycol, methyl-sulphoxide.The present invention recommends preferred organic solvent to be selected from following one or both and reaches above arbitrary combination: sherwood oil, hexanaphthene, ether, ethyl acetate, ethanol.
8. a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously as claimed in claim 1, it is characterized in that described be used for wash-out caffeine and chlorophyllous consumption of organic solvent be tea quality 1-20 doubly, divide 1-10 wash-out, the more preferably consumption of organic solvent that the present invention recommends is 4-10 times, and the preferred wash-out number of times that the present invention recommends is 2-5 time.
9. a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously as claimed in claim 1, it is characterized in that described organic solvent wash-out caffeine and chlorophyllous each soak time are 1min-60min, the preferred stirring soak time that the present invention recommends is 5-15min.
10. a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously as claimed in claim 1, it is characterized in that described from caffeine and chlorophyll mixture the employing ordinary method of preparation caffeine can be selected from the combination of following one or both and above method: liquid-liquid extraction, Solid-Phase Extraction, subliming method, CO
2Supercritical extraction, the preferred preparation method that the present invention recommends is a subliming method.
11. a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously as claimed in claim 1, it is characterized in that described the tealeaves pressed powder behind decaffeination, chlorophyll, the extraction in the tea-polyphenol process, need add less water soaks into, amount of water be tea quality 1-5 doubly, the present invention recommend preferred amount of water be tea quality 1-3 doubly.
12. a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously as claimed in claim 1, it is characterized in that described the tealeaves pressed powder behind decaffeination, chlorophyll, the extraction in the tea-polyphenol process, need in the tea-leaf power of water infiltration, add acid for adjusting pH value, and make pH≤7, the used acid of adjusting pH value can be selected from following one or both and reach above arbitrary combination: sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, citric acid, it is phosphoric acid that the present invention recommends preferred acid.
13. a kind of mechanochemistry principle of utilizing as claimed in claim 1 is extracted caffeine simultaneously from tealeaves, the novel method of tea-polyphenol and tea polysaccharide, it is characterized in that described from decaffeination, extract in the tea-polyphenol process in the tealeaves pressed powder behind the chlorophyll, after adding water infiltration and adding acid for adjusting pH value, need to add organic solvent and soak the wash-out tea-polyphenol, the organic solvent that soaks the wash-out tea-polyphenol can be selected from following one or both and reach above arbitrary combination: sherwood oil, hexane, hexanaphthene, octane-iso, trifluoroacetic acid, trimethylpentane, pentamethylene, heptane, Butyryl Chloride, trieline, tetracol phenixin, trichlorotrifluoroethane, propyl ether, toluene, p-Xylol, chlorobenzene, orthodichlorobenzene, ether, benzene, isopropylcarbinol, methylene dichloride, ethylene dichloride, propyl carbinol, N-BUTYL ACETATE, propyl alcohol, mibk, tetrahydrofuran (THF), ethyl acetate, Virahol, chloroform, methyl ethyl ketone, dioxan, pyridine, acetone, Nitromethane 99Min., ethanol, acetate, acetonitrile, aniline, dimethyl formamide, methyl alcohol, ethylene glycol, methyl-sulphoxide, the present invention recommends preferred organic solvent to be selected from following one or both and above arbitrary combination: propyl carbinol, ether, ethyl acetate, acetone, ethanol, methyl alcohol.
14. a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously as claimed in claim 1, it is characterized in that described the tealeaves pressed powder behind decaffeination, chlorophyll, the extraction in the tea-polyphenol process, after adding water infiltration and adding acid for adjusting pH value, need to add the organic solvent soaking and stirring, the organic solvent quality that is used to stir immersion be tea quality 1-20 doubly, divide 1-10 soaking and stirring, it is 6-12 times that the present invention recommends preferred consumption of organic solvent, and preferred soaking and stirring number of times is 3-6 time.
15. a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously as claimed in claim 1, it is characterized in that described the tealeaves pressed powder behind decaffeination, chlorophyll, the extraction in the tea-polyphenol process, need to add the organic solvent soaking and stirring, each soaking and stirring time is 1min-60min, and it is 5-10min that the present invention recommends the preferred soaking and stirring time.
16. a kind of novel method of utilizing the mechanochemistry principle to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously from tealeaves as claimed in claim 1 is characterized in that described tea-polyphenol is further purified method and can be selected from following one or both methods and above arbitrary combination: liquid-liquid extraction method, precipitation by metallic ion method, solid phase extraction or CO
2Supercritical extraction.
17. a kind of novel method of utilizing the mechanochemistry principle from tealeaves, to extract caffeine, tea-polyphenol and tea polysaccharide simultaneously as claimed in claim 1, it is characterized in that described the tealeaves pressed powder after having extracted caffeine, chlorophyll and tea-polyphenol, the extraction in the tea polysaccharide process, need add 5-10 times of water again, 100 ℃ of lixiviates, the centrifuging and taking supernatant liquor, add 3 times of these supernatant liquor volume dehydrated alcohols precipitation tea polysaccharide 24h, centrifugal, get the dry tea polysaccharide that obtains of precipitation.
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