CN101830882A - Method for simultaneously preparing seven catechin monomers from tea leaves - Google Patents
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Abstract
The invention relates to a method for simultaneously preparing seven catechin monomers from tea leaves, comprising the following steps of extraction, filtration, ultrafiltration, reverse-osmosis concentration, polyamide column chromatography, high-speed reverse-flow chromatograph purification and separation, concentration and drying. In the method, low-grade tea leaves, leftovers-processed broken tea siftings and fresh leaves or dry leaves of summer and autumn tea rarely utilized at present are used as raw materials, no any chemical reaction exists in the whole process, solvents comprising ethyl acetate, chloroform and the like are not used, macroporous resin with controversial safety in residual components are also not used, and therefore, the safety of a product is greatly improved; meanwhile, the method adopts a membrane technique to filter and remove impurities and concentrate so that the energy saving is above 6 times greater than that of the traditional heating evaporation concentration; extracts does not need to be extracted and dried into tea polyphenol and are directly separated and purified by using a concentrated solution, and therefore, the method greatly simplifies a preparation process and reduces production cost; and the method can be used for simultaneously preparing seven valuable catechin monomers.
Description
Technical field
The invention belongs to the processing of farm products field of deep tea processing technology, especially a kind of method for preparing seven kinds of catechin monomers from tealeaves simultaneously.
Background technology
Belonging to flavanone alcohols (Flavonol) compound on tea catechin (catechins) chemical structure, is that (Green Tea Polyphenols, main active ingredient GTP) account for the 60-80% of GTP total mass to tea-polyphenol.GTP is the general name of catechin in the tealeaves, flavonoid, phenolic acids and anthocyan compound, accounts for the 15-30% of dry weight of tea leaves.At present, tea-polyphenol has been widely used in food (batching and additive), medicine, healthcare products, daily use chemicals (toothpaste, body wash, shampoo etc.), weaving, air conditioning purge.The latest study proves, might on more deep and wide aspect, make contributions human health.Make vaccine, anti-new type influenzas etc. such as Whooping cough as catechin.(CCTV reports-and according to Japanese Asahi Shimbun website on August 1st, 2009, Osaka, Japan university and the researchist of municipal health research center, Yokohama utilize a kind of green tea extract to develop a kind of novel Tamiflu a few days ago.This medicine is that the EGCG after the processing is sneaked in seasonal influenza or the avian influenza virus, is injected into the kidney cell of animal again, the infection ability of research virus.Topology discovery, the effect that EGCG after the processing the suppresses virus infection anti-influenza medicament oseltamivir phosphate that can match in excellence or beauty ...).
The tea catechin compound is the general name of a class material, remove free radical, anti-oxidant, radioprotective, hypotensive blood pressure and blood lipoid, antibiotic, prevention cardiovascular and cerebrovascular diseases, aspect such as anticancer is the strongest composition of biological activity in the tea-polyphenol.Higher, the active stronger catechin of content mainly contains seven kinds in the tealeaves: E-C, EGC, D-C, EGCG, ECG, GCG and CG, molecular structural formula see accompanying drawing 1.Wherein E-C, EGC and D-C are non-ester catechin, and EGCG, ECG, GCG and CG are ester catechin.
The significance of separating, prepare multiple catechin monomers is: the research unit of tea-polyphenol and the content that factory all needs every kind of catechin in the testing product are produced in (1) tealeaves deep processing, need a large amount of standard controls, and the at present domestic minority monomer such as EGCG that only can prepare, and purity is not high, and most of user have to buy offshore company's product; (2) new drug, functional foodstuff research and development often need to prove its dosage and effect from the chemical ingredients angle, need a large amount of high-purity catechin monomers; (3) cakes and sweetmeats product, tea drink the latest study proves, the non-ester catechin bitter taste is little and the ester catechin bitter taste is heavier, can regulate the ratio of various catechins after the technology of the present invention is used arbitrarily; (4) body metabolism studies have shown that, complicated catechin (being generally the ester type) after being metabolized to simple catechin (being generally non-ester-type) more readily digested absorb, therefore need different catechin compatibilities during at the product of various objectives purposes in exploitation.
At present, the research of tea-polyphenol, catechin has become one of the thermoelectricity in fields such as Tea Processing, medicine, healthcare products, daily use chemicals, and relevant their extraction, separation, purifying has many bibliographical informations.But Technology and realization means (equipment) are more backward, and are in the majority with traditional method, mostly use the toxic organic solvent, cause dissolvent residual, energy consumption height, poor product quality; The catechin separation and purification is mostly carried out at EGCG compound, and mostly from the tea-polyphenol product, uses expensive import parting material Sephadex-LH20." a kind of method of separating the multiple catechin monomers of preparation from tea-polyphenol or catechin mixed system " (application number CN200910042834.8) discloses a kind of method of separating the multiple catechin monomers of preparation from tea-polyphenol or catechin mixed system.This method intercepts, dodges formula evaporation concentration, drying crystalline with tea-polyphenol or catechin mixed system sample through pre-treatment, liquid chromatography separation, cut, promptly prepare catechin monomers, the pre-place of tea-polyphenol or catechin mixed system sample is that mass concentration is 0.4～1.2mg/ml, adjust pH to 3.5～5.5 adopt the macroporous adsorption resin chromatography post to remove caffeine then; Adopt the liquid chromatography separation and purification, the chromatographic system stationary phase is C18 column internal diameter 50～100mm, packing material size 20～60 μ m, moving phase is: 12%～18% low-carbon alcohol+0.5～3% weak acid+water 87.5-79.0% (v/v), 10～60p a post are depressed with described moving phase elution chromatography post; Described sudden strain of a muscle formula evaporating concentration process is: cut liquid is injected sudden strain of a muscle formula vaporizer, carry out evaporation concentration under the condition of keeping 35-65 ℃ of collection liquid temp, obtain 4 kinds of catechin monomers.Different fully with raw material of the present invention and agent technology feature.
China is Tea Production big country, and tealeaves (dry product) annual production has reached 1,400,000 tons, and its low and middle-grade tea, fannings account for more than 20%.The utilization of not gathering of more substantial summer autumn tea leaf is still arranged every year.Therefore the present invention will be significant to the deep processing and the increasing both production and income of human health and tealeaves.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who from tealeaves, extracts seven kinds of catechin monomers simultaneously, from being processed as starting point with the bright leaf of low-grade tealeaves or summer autumn tea or the utilization of cured leaf, raw material is through the superheated water Continuous Countercurrent Extraction, ultrafiltration membrane technique separates macromolecular substance such as polysaccharide, albumen, be concentrated to solid content through reverse osmosis membrane technology again and reach higher level, concentrated solution is directly gone up homemade polyamide column chromatography and is made caffeine, ester catechin and non-ester catechin obtain initial gross separation and become three stream parts, collecting the back respectively concentrates, the ester type separates through countercurrent chromatography respectively with non-ester catechin stream part, obtains E-C, EGC, D-C, EGCG, ECG, seven kinds of catechin monomers of GCG and CG.Identify through check of technical Analysis such as HPLC, UV, IR, LC-MS, NMR and structure, prove that the purity of seven kinds of catechin monomers all reaches massfraction more than 98%.This invention technology is energy-conservation, low-cost, green, the method for suitability for industrialized production efficiently.
Technical scheme of the present invention: a kind ofly prepare the method for seven kinds of catechin monomers simultaneously, comprise the steps: from tealeaves
(1) extract: adopting the bright leaf or the cured leaf of tankage fannings sheet, low-grade tea dry product or the summer autumn tea of Tea Processing is raw material.Employing is a solvent liquid through the pure water of purifying treatment, and solid-liquid ratio W/W=1: 6-20 is with the disposable extraction of adverse current continuous extracting device.Obtaining solid content is the tea extracting solution of 1.5-5%.
(2) filtration and ultrafiltration: above-mentioned tea extracting solution is removed physics impurity such as big fannings sheet, silt with the continuous filtration of vibratory screening apparatus formula strainer earlier; Separate macromolecular polysaccharide, albumen, tannin with the ultra-filtration membrane device again.Obtain ultrafiltration and see through liquid and trapped fluid.
(3) reverse osmosis concentration: above-mentioned ultrafiltration is seen through liquid concentrates through the reverse osmosis unit circulation, to solid content be 8-20%, concentrated solution.
(4) polyamide column chromatography: concentrated solution is added the height/internal diameter=5-20 that installs in advance: 1 polymeric amide chromatography post, be that the aqueous ethanolic solution of 1-45%, 46-85% and 86-99% carries out wash-out as eluent with pure water and volume percent successively, fraction collection different ethanol concentration eluate obtains collecting liquid K, D, E and F respectively.Respectively above-mentioned collection liquid D, E and F are concentrated or concentrating under reduced pressure through the reverse osmosis unit circulation, to solid content be 10-20%, must collect concentrated solution D ', E ' and F ', F ' mainly contains caffeine, through further concentrating, can obtain after the crystallization, drying the caffeine of purity 50～98%.
(5) high speed adverse current chromatogram purifies and separates:, collect concentrated solution D ' and mainly contain non-ester catechin E-C, EGC and D-C through the HPLC analyzing and testing.Collect concentrated solution E ' and mainly contain ester catechin EGCG, ECG, GCG and CG.With D ', E ' high speed adverse current chromatogram purifies and separates, from collect concentrated solution D ', isolate non-ester catechin respectively, from collect concentrated solution E ', isolate ester catechin, collect corresponding effluent liquid respectively.
(6) concentrate, dry: vacuum concentration is near dry and reclaim solvent respectively for the collection effluent liquid of the different components that step (5) is obtained, and recovered solvent is after distillation, rectifying separation and recycle.Various enriched materials after concentrating obtain E-C, EGC, D-C, EGCG, ECG, GCG and seven kinds of catechin monomers products of CG after vacuum or vacuum lyophilization.
(7) structure is identified: with above-mentioned seven kinds of catechin monomers that obtain through HPLC external standard method and marker method qualitative and quantitative analysis, and employing UV, IR, H-NMR and ESI-MS four spectrum analysis, the result shows their four spectrum analysis data and standard spectrum diagram data consistent, matches with corresponding catechin structure.
The characteristics that step (1) is extracted are that can to adopt the bright leaf of summer autumn tea or cured leaf be raw material.Employing is a solvent through the pure water of purifying treatment, solid-liquid ratio (W/W)=1: 6-20, and with the disposable extraction of adverse current continuous extracting device, obtaining solid content is the tea extracting solution of 1.5-5%.
Step (2) is filtered and the characteristics of ultrafiltration are to remove physics impurity such as big fannings sheet, silt with the continuous filtration of grading oscillating screen formula strainer earlier.Grading oscillating screen is the screen cloth that is of five storeys in the airtight stainless steel equipment, is respectively 20 orders, 30 orders, 60 orders, 80 orders, 100 orders or 120 orders from top to bottom.
The ultra-filtration membrane device adopts ceramic membrane, and molecular weight cut-off is 5000～10000Dalton, is used to separate macromolecular polysaccharide, albumen, tannin etc.
Step (3) is to adopt reverse osmosis concentration to replace present widely used normal pressure or reduction vaporization concentrates, to solid content be 8-20%, can save the energy (in price of coal and electricity) cost 60～80%.
Step (4) polyamide column chromatography is to adopt homemade chromatography polymeric amide parting material, and granularity is 30～200 orders.Height/the internal diameter of pillar=5-20: 1.Four kinds of eluents are respectively pure water, and volume percent concentration 1-45%, 46-85% and 86-99% ethanol-water solution.The consumption of every kind of eluent is a 2-5 times of column volume (BV).
Step (5) high speed adverse current chromatogram purifies and separates, chromatographic condition is that PTFE is that (the liquid loading capacity can 0.5-500L for tetrafluoroethylene material tubing string, one time applied sample amount can reach 0.5-1000g), it is n-butanol-water (V/V=1/3-3/1) that the preparation of non-ester catechin E-C, EGC and D-C separates solvent systems.It is ethyl acetate-water (V/V=1/3-3/1) that the preparation of ester catechin EGCG, ECG, GCG and CG separates solvent systems.
Adopt the beneficial effect of technique scheme to be:
The present invention adopts and keeps out time tealeaves, the bright leaf or the cured leaf of processing fent fannings sheet and the existing summer autumn tea that also seldom utilizes are raw material, whole technological process is without any chemical reaction, do not use ethyl acetate, chloroform equal solvent, do not use controversial macroporous resin on residual component safety yet, Product Safety is improved greatly; Simultaneously, adopt the membrane technique filtering and impurity removing, concentrate, concentrate energy-conservation more than 60% than traditional heating evaporation; Do not need the extract extraction, be dried to tea-polyphenol, but, simplified preparation technology greatly, reduced production cost with the direct separation and purification of concentrated solution; Can prepare 7 kinds of valuable catechin monomers simultaneously.
Embodiment
Below provide embodiment, the invention will be further described.
Embodiment 1
(1) extract: getting the tankage fannings sheet 1000g of Green Tea Processing, is solvent with 8000g through the pure water of purifying treatment, with the disposable extraction of pillar adverse current continuous extracting device.Obtain solid content and be 4.3% tea extracting solution 7000g.
(2) filtration and ultrafiltration: above-mentioned tea extracting solution is removed physics impurity such as big fannings sheet, silt with the continuous filtration of vibratory screening apparatus formula strainer earlier; Separate macromolecular polysaccharide, albumen, tannin etc. with the ultra-filtration membrane device again.Obtain the 6300g ultrafiltration and see through liquid A and 700g trapped fluid B.
(3) reverse osmosis concentration: above-mentioned ultrafiltration is seen through liquid A concentrates through the reverse osmosis unit circulation, to solid content be 20%, 1250g concentrated solution C.
(4) polyamide column chromatography: 100g concentrated solution C is added height/internal diameter=10: the 1 polymeric amide chromatography posts that install in advance, and the polyamide granules degree is 150 orders, and bed volume is 1000mL.Be that 15%, 50% and 90% aqueous ethanolic solution carries out wash-out as eluent with the pure water volume fraction successively, every kind of eluent consumption is 3BV.Fraction collection different ethanol concentration eluate obtains collecting liquid K, D, E and F respectively.Mainly contain water-soluble impurities such as polysaccharide, albumen among the K, discard.Respectively above-mentioned collection liquid D is concentrated through the reverse osmosis unit circulation, E and F are through concentrating under reduced pressure, and vacuum tightness is that 0.06-0.02MPa is 20% to solid content, and the recovery solvent gets concentrated solution D ', E ' and F '.F ' mainly contains caffeine, through further concentrating, obtain behind the alcohol crystal, 80 dryings the caffeine of purity 95%.
(5) high speed adverse current chromatogram purifies and separates: with D ' high speed adverse current chromatogram purifies and separates, chromatographic condition be PTFE (tetrafluoroethylene) material tubing string (
One time applied sample amount can reach 5g), it is n-butanol-water (V/V=1: 1.5) that preparation separates solvent systems.Collect corresponding non-ester catechin E-C, EGC, a D-C3 peak effluent liquid respectively.
E ' high speed adverse current chromatogram purifies and separates, chromatographic condition be PTFE (tetrafluoroethylene) material tubing string (
One time applied sample amount can reach 5g), it is ethyl acetate-water (V/V=1.5: 1) that preparation separates solvent systems.Collect the effluent liquid at four peaks of ester catechin EGCG, ECG, GCG and CG correspondence respectively.
(6) concentrate, dry: the collection liquid of the different components that will (5) obtains respectively vacuum concentration to being close to dry and reclaiming solvent, recovered solvent through distill, after the rectifying separation and recycle.Various enriched materials obtain E-C, EGC, D-C, EGCG, ECG, GCG and seven kinds of catechin monomers products of CG through 55 ℃ of vacuum (0.01-0.005MPa) drying.Total recovery rate is 75-80% (calculating with initial content in the tea raw material).
(7) structure is identified: with above-mentioned seven kinds of catechin monomers that obtain through HPLC external standard method and marker method qualitative and quantitative analysis, and employing UV, IR, H-NMR and ESI-MS four spectrum analysis, the result shows their four spectrum analysis data and standard spectrum diagram data consistent, matches with corresponding catechin structure.Purity is all greater than 98.0%.
Embodiment 2
(1) extract: get the bud green tealeaves 2000g (being equivalent to about cured leaf 500g) in August, chopping is solvent with 10000g through the pure water of purifying treatment, with the disposable extraction of ring type adverse current continuous extracting device.Obtain solid content and be 1.5% tea extracting solution 10000g.
(2) filtration and ultrafiltration: above-mentioned tea extracting solution is removed physics impurity such as big fannings sheet, silt with the continuous filtration of vibratory screening apparatus formula strainer earlier; Separate macromolecular polysaccharide, albumen, tannin etc. with the ultra-filtration membrane device again.Obtain the 9500g ultrafiltration and see through liquid A and trapped fluid B.
(3) reverse osmosis concentration: above-mentioned ultrafiltration is seen through liquid A concentrates through the reverse osmosis unit circulation, to solid content be 20%, 625g concentrated solution C.
(4) polyamide column chromatography: 100g concentrated solution C is added height/internal diameter=15: the 1 polymeric amide chromatography posts that install in advance, and the polyamide granules degree is 120 orders, and bed volume is 1000mL.Be that 0,10%, 55% and 95% aqueous ethanolic solution carries out wash-out as eluent with volume fraction successively, every kind of eluent consumption is 2.5BV.Fraction collection different ethanol concentration eluate obtains collecting liquid K, D, E and F respectively.Mainly contain water-soluble impurities such as polysaccharide, albumen among the K, discard.Respectively above-mentioned collection liquid D is concentrated through the reverse osmosis unit circulation, E and F are through concentrating under reduced pressure, and vacuum tightness is that 0.07-0.01MPa is 20% to solid content, and the recovery solvent gets concentrated solution D ', E ' and F '.F ' mainly contains caffeine, through further concentrating, can obtain behind the alcohol crystal, 80 dryings the caffeine of purity 95%.
(5) high speed adverse current chromatogram purifies and separates: with D ' high speed adverse current chromatogram purifies and separates, chromatographic condition be PTFE (tetrafluoroethylene) material tubing string (
One time applied sample amount can reach 10g), it is n-butanol-water (V/V=1.5: 1.0) that preparation separates solvent systems.Collect corresponding non-ester catechin E-C, EGC, a D-C3 peak effluent liquid respectively.
E ' high speed adverse current chromatogram purifies and separates, chromatographic condition be PTFE (tetrafluoroethylene) material tubing string (
One time applied sample amount can reach 10g), it is ethyl acetate-water (V/V=2.0: 1) that preparation separates solvent systems.Collect the effluent liquid at four peaks of ester catechin EGCG, ECG, GCG and CG correspondence respectively.
(6) concentrate, dry: the collection liquid of the different components that will (5) obtains respectively vacuum concentration to being close to dry and reclaiming solvent, recovered solvent through distill, after the rectifying separation and recycle.Various enriched materials obtain E-C, EGC, D-C, EGCG, ECG, GCG and seven kinds of catechin monomers products of CG through vacuum (0.001-0.005MPa) lyophilize (30--20 ℃).Total recovery rate is 75-80% (calculating with initial content in the tea raw material).
(7) structure is identified: with above-mentioned seven kinds of catechin monomers that obtain through HPLC external standard method and marker method qualitative and quantitative analysis, and employing UV, IR, H-NMR and ESI-MS four spectrum analysis, the result shows their four spectrum analysis data and standard spectrum diagram data consistent, matches with corresponding catechin structure.Purity is all greater than 98.0%.
Claims (6)
1. one kind prepares the method for seven kinds of catechin monomers simultaneously from tealeaves, and it is characterized in that: it adopts following several steps:
Extract: adopting the bright leaf or the cured leaf of tankage fannings sheet, low-grade tea or the summer autumn tea of Tea Processing is raw material, employing is a solvent liquid through the pure water of purifying treatment, solid-liquid ratio W/W=1: 6-20, with the disposable extraction of adverse current continuous extracting device, obtaining solid content is the tea extracting solution of 1.5-5%;
Filter and ultrafiltration: above-mentioned tea extracting solution is removed impurity such as bigger fannings sheet, silt with the continuous filtration of vibratory screening apparatus formula strainer earlier; Separate with the ultra-filtration membrane device again and remove macromolecular polysaccharide, albumen, tannin, obtain ultrafiltration and see through liquid and trapped fluid;
Reverse osmosis concentration: above-mentioned ultrafiltration is seen through liquid concentrates through the reverse osmosis unit circulation, to solid content be 8-20%, concentrated solution;
Polyamide column chromatography: concentrated solution is added the height/internal diameter=5-20 that installs in advance: 1 polymeric amide chromatography post, water and concentration are that volume percent is that the aqueous ethanolic solution of 1-45%, 46-85%, 86-99% carries out wash-out as eluent successively, fraction collection different ethanol concentration eluate obtains collecting liquid K, D, E and F respectively; Mainly contain water-soluble impurities such as polysaccharide, albumen among the K, discard, respectively above-mentioned collection liquid D, E and F are concentrated or reduction vaporization concentrates through the reverse osmosis unit circulation, to solid content be 10-20%, must collect concentrated solution D ', E ' and F '; Collect concentrated solution F ' and mainly contain caffeine, through further concentrating, obtain after the crystallization, drying the caffeine of purity 50-98%;
High speed adverse current chromatogram purifies and separates: through the HPLC analyzing and testing, collect concentrated solution D ' and mainly contain non-ester catechin E-C, EGC and D-C, collect concentrated solution E ' and mainly contain ester catechin EGCG, ECG, GCG and CG; To collect concentrated solution D ', E ' high speed adverse current chromatogram purifies and separates respectively, to isolate non-ester catechin E-C among the concentrated solution D ', EDC and DC isolate several effluent liquid of ester catechin EGCG, ECG, GCG and CG from collect concentrated solution E ', collect corresponding effluent liquid more respectively;
Concentrate, dry: the effluent liquid that regathers of the different components that purifies and separates is obtained respectively vacuum concentration near dry and reclaim solvent, recovered solvent is through distillation, after the rectifying separation and recycle, and the various enriched materials after concentrated obtain E-C, EGC, D-C, EGCG, ECG, GCG and seven kinds of catechin monomers products of CG again after vacuum or vacuum lyophilization.
2. according to claim 1ly a kind ofly prepare the method for seven kinds of catechin monomers simultaneously from tealeaves, it is characterized in that: the characteristics that step is extracted are that to adopt the bright leaf of summer autumn tea or cured leaf be raw material.
3. according to claim 1ly a kind ofly prepare the method for seven kinds of catechin monomers simultaneously, it is characterized in that: filter and the characteristics of ultrafiltration are to remove physics impurity such as bigger fannings sheet, silt with the continuous filtration of grading oscillating screen formula strainer earlier from tealeaves; Grading oscillating screen is an airtight stainless steel equipment, and the screen cloth that wherein is of five storeys, its screen cloth are respectively 20 orders, 30 orders, 60 orders, 80 orders, 100 orders or 120 orders from top to bottom; The ultra-filtration membrane device adopts ceramic membrane ultrafitration equipment.
4. according to claim 1ly a kind ofly prepare the method for seven kinds of catechin monomers simultaneously, it is characterized in that from tealeaves: adopt reverse osmosis concentration to replace evaporation concentration, to solid content be 8-20%.
5. according to claim 1ly a kind ofly prepare the method for seven kinds of catechin monomers simultaneously from tealeaves, it is characterized in that: described polyamide column chromatography is to adopt homemade chromatography polymeric amide parting material, and granularity is the 30-200 order, the height/internal diameter of pillar=5-20: 1; Four kinds of eluents are respectively pure water, and the concentration volume percent is the aqueous ethanolic solution of 1-45%, 46-85% and 86-99%; The consumption of every kind of eluent is 2-5 times of column volume BV.
6. a kind of method for preparing seven kinds of catechin monomers from tealeaves simultaneously according to claim 1, it is characterized in that: the high speed adverse current chromatogram purifies and separates, chromatographic condition is that PTFE is a tetrafluoroethylene material tubing string, it is n-butanol-water that the preparation of non-ester catechin E-C, EGC and D-C separates solvent systems, V/V=1/3-3/1; It is ethyl acetate-water V/V=1/3-3/1 that the preparation of ester catechin EGCG, ECG, GCG and CG separates solvent systems.
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| CN105866342A (en) * | 2016-05-13 | 2016-08-17 | 中国农业科学院茶叶研究所 | Method for quickly detecting biochemical components of fresh tea leaf sample |
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