CN108619323A - The technique for isolating and purifying tea polyphenols using tea grounds - Google Patents
The technique for isolating and purifying tea polyphenols using tea grounds Download PDFInfo
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- CN108619323A CN108619323A CN201810671194.6A CN201810671194A CN108619323A CN 108619323 A CN108619323 A CN 108619323A CN 201810671194 A CN201810671194 A CN 201810671194A CN 108619323 A CN108619323 A CN 108619323A
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- 241001122767 Theaceae Species 0.000 title claims abstract description 159
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 125
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 125
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000002525 ultrasonication Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 88
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 72
- 239000002002 slurry Substances 0.000 claims description 67
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 54
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 claims description 45
- 229940043264 dodecyl sulfate Drugs 0.000 claims description 45
- 238000000605 extraction Methods 0.000 claims description 45
- 235000019441 ethanol Nutrition 0.000 claims description 44
- 239000012043 crude product Substances 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- 239000012530 fluid Substances 0.000 claims description 41
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 229950008882 polysorbate Drugs 0.000 claims description 27
- 229920000136 polysorbate Polymers 0.000 claims description 27
- 235000011837 pasties Nutrition 0.000 claims description 25
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- 238000000926 separation method Methods 0.000 claims description 14
- 238000010521 absorption reaction Methods 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 13
- 229920005989 resin Polymers 0.000 claims description 13
- 244000062793 Sorghum vulgare Species 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 12
- 235000019713 millet Nutrition 0.000 claims description 12
- 239000011148 porous material Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- 239000008236 heating water Substances 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 238000001694 spray drying Methods 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000003480 eluent Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- 238000010936 aqueous wash Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 150000002148 esters Chemical class 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 2
- 239000005864 Sulphur Substances 0.000 claims 2
- 239000011734 sodium Substances 0.000 claims 2
- 229910052708 sodium Inorganic materials 0.000 claims 2
- 239000000284 extract Substances 0.000 abstract description 13
- 238000011084 recovery Methods 0.000 abstract description 12
- 229940093499 ethyl acetate Drugs 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 11
- 238000011017 operating method Methods 0.000 description 10
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 9
- 239000000126 substance Substances 0.000 description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 description 4
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 125000004494 ethyl ester group Chemical group 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 description 2
- CITFYDYEWQIEPX-UHFFFAOYSA-N Flavanol Natural products O1C2=CC(OCC=C(C)C)=CC(O)=C2C(=O)C(O)C1C1=CC=C(O)C=C1 CITFYDYEWQIEPX-UHFFFAOYSA-N 0.000 description 2
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 2
- 229960001948 caffeine Drugs 0.000 description 2
- 235000005487 catechin Nutrition 0.000 description 2
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 2
- 229950001002 cianidanol Drugs 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000011987 flavanols Nutrition 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 239000002075 main ingredient Substances 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- LSHVYAFMTMFKBA-TZIWHRDSSA-N (-)-epicatechin-3-O-gallate Chemical compound O([C@@H]1CC2=C(O)C=C(C=C2O[C@@H]1C=1C=C(O)C(O)=CC=1)O)C(=O)C1=CC(O)=C(O)C(O)=C1 LSHVYAFMTMFKBA-TZIWHRDSSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 102000003992 Peroxidases Human genes 0.000 description 1
- CIOAGBVUUVVLOB-NJFSPNSNSA-N Strontium-90 Chemical compound [90Sr] CIOAGBVUUVVLOB-NJFSPNSNSA-N 0.000 description 1
- 102000003425 Tyrosinase Human genes 0.000 description 1
- 108060008724 Tyrosinase Proteins 0.000 description 1
- 229930002877 anthocyanin Chemical class 0.000 description 1
- 239000004410 anthocyanin Chemical class 0.000 description 1
- 235000010208 anthocyanin Nutrition 0.000 description 1
- 150000004636 anthocyanins Chemical class 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000001185 bone marrow Anatomy 0.000 description 1
- 239000001058 brown pigment Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002206 flavan-3-ols Chemical class 0.000 description 1
- -1 flavanol compound Chemical class 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- HVQAJTFOCKOKIN-UHFFFAOYSA-N flavonol Chemical class O1C2=CC=CC=C2C(=O)C(O)=C1C1=CC=CC=C1 HVQAJTFOCKOKIN-UHFFFAOYSA-N 0.000 description 1
- 150000002216 flavonol derivatives Chemical class 0.000 description 1
- 235000011957 flavonols Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 108040007629 peroxidase activity proteins Proteins 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000941 radioactive substance Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000037394 skin elasticity Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/82—Theaceae (Tea family), e.g. camellia
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Botany (AREA)
- Mycology (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medical Informatics (AREA)
- Epidemiology (AREA)
- Food Science & Technology (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Nutrition Science (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Pharmacology & Pharmacy (AREA)
- Polymers & Plastics (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Non-Alcoholic Beverages (AREA)
Abstract
The invention discloses a kind of techniques isolating and purifying tea polyphenols using tea grounds, belong to tea polyphenol extract technical field.The technique that tea polyphenols are isolated and purified using tea grounds includes tea grounds feedstock processing, ultrasonication, supercritical CO2It extracts, isolate and purify.Technique using the present invention isolates and purifies tea polyphenols, the recovery rate and purity of tea polyphenols can be improved, to increase economic efficiency.
Description
Technical field
The invention belongs to tea polyphenol extract technical fields, and in particular to the technique for isolating and purifying tea polyphenols using tea grounds.
Background technology
Tea polyphenols（Tea Polyphenols）It is the general name of Polyphenols of Tea, including flavanol compound, anthocyanin
Class, flavonoids, flavonols and phenolic acid class etc..Predominantly flavanols（Catechin）Class, catechin account for 60 ~ 80%.Tea polyphenols are also known as
Tea tan or tea tannin, be have in one of main ingredient to form tealeaves color, smell and taste and tealeaves healthcare function main ingredient it
One.Studies have shown that the removing toxic substances of tea polyphenols isoreactivity substance tool and radiation resistance, can effectively stop radioactive substance intrusion bone
Marrow, and strontium 90 and Co 60 can be made to excrete rapidly, it is described as " radiation jinx " by health and medical field.
Tea polyphenols have very strong antioxidation, have inhibiting effect to clostridiopetidase A and elastoser, can prevent elasticity
The content of albumen declines or denaturation, maintains skin elasticity, reaches wrinkle-proof effect.Tea polyphenols can absorb ultraviolet light, reduce melanin
Growth, have inhibiting effect to tyrosinase and peroxidase, to reach whitening function.Polyphenol is one kind in ultraviolet area
There is the natural products of strong absorbent, and to human body nontoxicity.By the compounding of several polyphenol and flavones, its ultraviolet region is utilized
The sun-proof composite natural ultraviolet absorbent of wide spectrum can be obtained in the difference of absorption, plays the formation for reducing dermal melanin, prevents skin old
The effect of change.
Tea grounds is remaining tea waste after the processes such as tealeaves is extracted, impregnates, and contains 1 ~ 6% tea in tea grounds toward contact
Polyphenol.And the tea grounds number that the industrialization extraction of tealeaves generates every year is considerable, therefore, extraction tea polyphenols have from tea grounds
Realistic meaning.
Traditional tea polyphenol extract uses solvent extraction, and tea polyphenol extract rate is low (general recovery rate is 5%-6%), product
Purity is low, and product is oxidizable, and wherein contains a large amount of impurities (such as plant polyose, tea brown pigment, pigment, caffeine, resin).
It is extracted with organic solvent, though recovery rate can increase and (can reach 1O%-15%), and it is more due to not only containing tea in leaching liquor
Phenol, but also containing the impurity such as Tea Pigment, caffeine, to obtain fine work, must also impurity removal and purification repeatedly, process is more, and technique is cumbersome
Complexity, extraction process generally need to be through 3 grades of cross current solvent extractions；It need to repeatedly distill, heating time is long；It needs with a large amount of organic solvent,
Some organic solvent recycling are difficult, toxic, inflammable, are unfavorable for keeping the safety in production.
Invention content
The purpose of the present invention is to provide a kind of techniques isolating and purifying tea polyphenols using tea grounds, to solve tea polyphenol extract
Rate and the low problem of purity.
In order to solve the above technical problems, the present invention uses following technical scheme：
The technique that tea polyphenols are isolated and purified using tea grounds, is included the following steps：
S1, tea grounds feedstock processing；
S2, ultrasonication；
S3, supercritical CO2Extraction；
S4, it isolates and purifies；
The tea grounds feedstock processing, includes the following steps：
Tea grounds is dried and is ground into 120-200 mesh, then adds distilled water, be placed in vacuum high shear homogenizer fully it is homogeneous,
Water pasty slurry is obtained, heating water bath is then used, makes the control of water pasty slurry temperature at 60-65 DEG C, and in water pasty slurry
Middle addition ethyl alcohol stirs 10-25min with the speed of 200-500r/min, and slurries, the tea grounds are obtained after placing cooling 0.4-0.9h
Amount ratio with distilled water is 1:The amount ratio of 10-15, a concentration of 34%-38% of the ethyl alcohol, tea grounds and ethyl alcohol is 1:0.5-
0.8。
Further, ultrasonication described in step S2 is to carry out ultrasonication to slurries, and the slurries of processing are made,
The frequency of the ultrasonic wave is 25-30KHz, processing time 5-8min.
Further, supercritical CO described in step S32Extraction, includes the following steps：
The slurries handled through step S2 are used into supercritical CO2Extraction, in CO2Sldium lauryl sulfate, acetic acid second are added in fluid
Ester, polysorbate, control extracting pressure are 26-30MPa, and extraction temperature is 52-58 DEG C, CO2Flow is 20-25L/h, when extraction
Between be 1.5-3.5h, obtain tea polyphenols crude product a, tea polyphenols crude product detached with slurries, separating pressure 3-6Mpa, separation temperature
It is 40-50 DEG C；Remaining slurries use supercritical CO again2Extraction, in CO2Acetone, sldium lauryl sulfate, control are added in fluid
Extracting pressure is 22-27MPa, and extraction temperature is 50-56 DEG C, CO2Flow is 20-25L/h, and extraction time 1-2h obtains tea
Polyphenol crude product b detaches tea polyphenols crude product with slurries, separating pressure 3-6Mpa, and separation temperature is 40-50 DEG C, by gained tea
Polyphenol crude product a and the b mixing of tea polyphenols crude product, add hydrochloric acid, adjusting pH value is 3-5.2, centrifuges or is separated by filtration, obtains millet paste；
Further, the sldium lauryl sulfate, ethyl acetate, polysorbate total dosage be CO2The 15%-24% of fluid,
Middle sldium lauryl sulfate, ethyl acetate, polysorbate weight proportion be（1.2-2.5）:（0.6-2）:（1.5-3）.
Further, the sldium lauryl sulfate, ethyl acetate, polysorbate weight proportion be 1.8:2:2.6.
Further, the acetone, sldium lauryl sulfate total dosage be CO2The 12%-18% of fluid, wherein acetone, the moon
The weight proportion of lauryl sulfate is（1-2）：（0.4-0.9）.
Further, the acetone, sldium lauryl sulfate weight proportion be 1.6:0.8.
Further, a concentration of 18%-28% of the hydrochloric acid, dosage are the 6%-16% of tea polyphenols crude product total amount.
Further, it isolates and purifies, includes the following steps described in step S4：
Blade diameter length ratio by LX-8 types large pore resin absorption column on millet paste, LX-8 type large pore resin absorption columns is 1:5-15, applied sample amount
It it is 37-56 times of column volume, loading flow velocity is 0 .5-2 BV/h, the ethanol aqueous wash for being first 1.2-7.5% with volume fraction
Remove miscellaneous, dosage is 20-26 times of column volume, flow velocity is 1-4 BV/h, then with volume fraction be 56%-73% ethyl alcohol it is water-soluble
Liquid elutes, and dosage is 12-18 times of column volume, flow velocity is 1-4 BV/h, and collected volume score is that the ethyl alcohol of 56%-73% is water-soluble
The eluent of liquid is concentrated under reduced pressure, and spray drying is dry, and tea polyphenols product is made.
Further, dry described in step S4 is spray drying or freeze-drying.
The invention has the advantages that：
（1）By the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment, tea polyphenol extract rate and purity highest are obtained.
（2）By embodiment 2 and the data of comparative example 1-4 as it can be seen that step S1 adds ethyl alcohol in water pasty slurry, with
The operating procedure of the speed stirring 10mi of 500r/min；Lack in CO in step S32CO is added in fluid2The moon of fluid volume 15%
The operating procedure of lauryl sulfate, ethyl acetate, polysorbate；Lack addition hydrochloric acid in step S3, adjusts the behaviour that pH value is 4.8
Make step, synergistic effect is played during extracting tea polyphenols, collaboration improves the recovery rate and purity of tea polyphenols；This
It is：
Ethyl alcohol is added in step S1 in water pasty slurry, the ethyl alcohol of addition is polar solvent, and tea polyphenols are also polar substances, root
According to the principle of similar compatibility, ethyl alcohol can promote the dissolution of tea polyphenols in water, the dissolution without influencing other apolar substances
Rate；Heating water bath and 10mi is stirred with the speed of 500r/min simultaneously so that tea grounds internal temperature increases, and stirring can accelerate tea more
The diffusion of the extracts such as phenol, and then tea polyphenols is made quickly to be leached out, to increase the recovery rate and purity of tea polyphenols.Due to tea
Polyphenol is in CO2Solubility in fluid is little, causes its recovery rate not high, and the present invention lives according to sldium lauryl sulfate with surface
Change performance, solution can be made fully to activate, the characteristics of tea polyphenols are soluble in ethyl acetate and polysorbate can be as solubilizer
Micelle is formed in water, Adsorption of Tea Polyphenols substance and increase tea polyphenols in CO2The features such as solubility in fluid, in step s3 to
CO2CO is added in fluid2Sldium lauryl sulfate, ethyl acetate, the polysorbate of fluid volume 15%, it is possible to increase tea polyphenols are in CO2
Solubility in fluid；On the basis of adding ethyl alcohol into water pasty slurry in step sl, have in conjunction with sldium lauryl sulfate
Surfactant property can be such that solution fully activates and the characteristics of tea polyphenols are soluble in ethyl acetate, further increase tea polyphenols
Recovery rate.Tea polyphenols are stablized in acid condition, oxidizable under alkaline condition, and step S3 adds after tea polyphenol extract separation
Add acetic acid, it is 4.8 to adjust pH value, can prevent tea polyphenols from being aoxidized, to improve the purity of tea polyphenols.
Specific implementation mode
In order to better understand the present invention, it is first illustrated using following implementation, following embodiment belongs to the present invention
Protection domain, but do not limit the scope of the invention.
The technique that tea polyphenols are isolated and purified using tea grounds, is included the following steps：
S1：Tea grounds is dried and is ground into 120-200 mesh, then adds distilled water, is placed in vacuum high shear homogenizer fully even
Matter obtains water pasty slurry, then uses heating water bath, makes the control of water pasty slurry temperature at 60-65 DEG C, and is starched in water paste
Ethyl alcohol is added in material, 10-25min is stirred with the speed of 200-500r/min, and slurries, the tea are obtained after placing cooling 0.4-0.9h
The amount ratio of slag and distilled water is 1:The amount ratio of 10-15, a concentration of 34%-38% of the ethyl alcohol, tea grounds and ethyl alcohol is 1:
0.5-0.8；
S2：Ultrasonication is carried out to slurries, the frequency of the ultrasonic wave is 25-30KHz, processing time 5-8min, is made
The slurries of processing；
S3：The slurries handled through step S2 are used into supercritical CO2Extraction, in CO2Sldium lauryl sulfate, acetic acid are added in fluid
Ethyl ester, polysorbate, the sldium lauryl sulfate, ethyl acetate, polysorbate total dosage be CO2The 15%-24% of fluid,
Middle sldium lauryl sulfate, ethyl acetate, polysorbate weight proportion be（1.2-2.5）:（0.6-2）:（1.5-3）, control extraction
Pressure power is 26-30MPa, and extraction temperature is 52-58 DEG C, CO2Flow is 20-25L/h, and extraction time 1.5-3.5h is obtained
Tea polyphenols crude product a detaches tea polyphenols crude product with slurries, separating pressure 3-6Mpa, and separation temperature is 40-50 DEG C；Residue slurry
Liquid uses supercritical CO again2Extraction, in CO2Acetone, sldium lauryl sulfate, the acetone, sldium lauryl sulfate are added in fluid
Total dosage be CO2The 12%-18% of fluid, wherein acetone, sldium lauryl sulfate weight proportion be（1-2）：（0.4-0.9）,
Control extracting pressure is 22-27MPa, and extraction temperature is 50-56 DEG C, CO2Flow is 20-25L/h, and extraction time 1-2h is obtained
To tea polyphenols crude product b, tea polyphenols crude product is detached with slurries, separating pressure 3-6Mpa, separation temperature is 40-50 DEG C, by institute
Tea polyphenols crude product a and the b mixing of tea polyphenols crude product are obtained, adds hydrochloric acid, a concentration of 18%-28% of the hydrochloric acid, dosage is tea polyphenols
The 6%-16% of crude product total amount, adjusting pH value are 3-5.2, centrifuge or are separated by filtration, obtain millet paste；
S4：Blade diameter length ratio by LX-8 types large pore resin absorption column on millet paste, LX-8 type large pore resin absorption columns is 1:5-15, loading
Amount is 37-56 times of column volume, and loading flow velocity is 0 .5-2 BV/h, the ethanol water for being first 1.2-7.5% with volume fraction
Elution removal of impurities, dosage is 20-26 times of column volume, flow velocity is 1-4 BV/h, then the ethanol water for being 56%-73% with volume fraction
Solution elutes, and dosage is 12-18 times of column volume, flow velocity is 1-4 BV/h, and collected volume score is the ethanol water of 56%-73%
The eluent of solution is concentrated under reduced pressure, and tea polyphenols product is made in spray drying or freeze-drying.
Embodiment 1
A kind of technique being isolated and purified tea polyphenols using tea grounds, is included the following steps：
S1：Tea grounds is dried and is ground into 180 mesh, then adds distilled water, be placed in vacuum high shear homogenizer fully it is homogeneous, obtain
To water pasty slurry, heating water bath is then used, makes the control of water pasty slurry temperature at 62 DEG C, and added in water pasty slurry
Ethyl alcohol stirs 10min with the speed of 500r/min, and slurries, the amount ratio of the tea grounds and distilled water are obtained after placing cooling 0.6h
It is 1:12, a concentration of the 36% of the ethyl alcohol, the amount ratio of tea grounds and ethyl alcohol is 1:0.7；
S2：Ultrasonication is carried out to slurries, the frequency of the ultrasonic wave is 30KHz, processing time 5min, and processing is made
Slurries；
S3：The slurries handled through step S2 are used into supercritical CO2Extraction, in CO2Sldium lauryl sulfate, acetic acid are added in fluid
Ethyl ester, polysorbate, the sldium lauryl sulfate, ethyl acetate, polysorbate total dosage be CO2The 22% of fluid, the wherein moon
Lauryl sulfate, ethyl acetate, polysorbate weight proportion be 1.8:2:2.6, control extracting pressure is 28MPa, extraction temperature
Degree is 56 DEG C, CO2Flow is 23L/h, extraction time 2.5h, obtains tea polyphenols crude product a, by tea polyphenols crude product and slurries point
From separating pressure 5Mpa, separation temperature is 45 DEG C；Remaining slurries use supercritical CO again2Extraction, in CO2It is added in fluid
Acetone, sldium lauryl sulfate, the acetone, sldium lauryl sulfate total dosage be CO2The 15% of fluid, wherein acetone, laruyl alcohol
The weight proportion of sodium sulphate is 1.6:0.8, control extracting pressure is 25MPa, and extraction temperature is 55 DEG C, CO2Flow is 22L/h,
Extraction time is 1.5h, obtains tea polyphenols crude product b, tea polyphenols crude product is detached with slurries, separating pressure 5Mpa, separation temperature
It is 46 DEG C, gained tea polyphenols crude product a and tea polyphenols crude product b is mixed, adds hydrochloric acid, a concentration of the 25% of the hydrochloric acid, dosage is
The 20% of tea polyphenols crude product total amount, it is 4.8 to adjust pH value, centrifuges or is separated by filtration, obtains millet paste；
S4：Blade diameter length ratio by LX-8 types large pore resin absorption column on millet paste, LX-8 type large pore resin absorption columns is 1:10, applied sample amount
It it is 50 times of column volume, loading flow velocity is 1.5 BV/h, first uses the ethanol aqueous wash removing that volume fraction is 5.2% miscellaneous, uses
Amount is 23 times of column volume, flow velocity is 3 BV/h, then the ethanol water for being 65% with volume fraction elutes, and dosage is cylinder
Long-pending 15 times, flow velocity be 3 BV/h, the eluent for the ethanol water that collected volume score is 65% is concentrated under reduced pressure, spray drying
Or freeze-drying, tea polyphenols product is made.
Embodiment 2
A kind of technique being isolated and purified tea polyphenols using tea grounds, is included the following steps：
S1：Tea grounds is dried and is ground into 120 mesh, then adds distilled water, be placed in vacuum high shear homogenizer fully it is homogeneous, obtain
To water pasty slurry, heating water bath is then used, makes the control of water pasty slurry temperature at 60 DEG C, and added in water pasty slurry
Ethyl alcohol stirs 22min with the speed of 300r/min, and slurries, the amount ratio of the tea grounds and distilled water are obtained after placing cooling 0.5h
It is 1:10, a concentration of the 34% of the ethyl alcohol, the amount ratio of tea grounds and ethyl alcohol is 1:0.8；
S2：Ultrasonication is carried out to slurries, the frequency of the ultrasonic wave is 25KHz, processing time 8min, and processing is made
Slurries；
S3：The slurries handled through step S2 are used into supercritical CO2Extraction, in CO2Sldium lauryl sulfate, acetic acid are added in fluid
Ethyl ester, polysorbate, the sldium lauryl sulfate, ethyl acetate, polysorbate total dosage be CO2The 15% of fluid, the wherein moon
Lauryl sulfate, ethyl acetate, polysorbate weight proportion be 1.2:0.8:2.6, control extracting pressure is 26MPa, extraction
Temperature is 52 DEG C, CO2Flow is 25L/h, extraction time 3.5h, obtains tea polyphenols crude product a, by tea polyphenols crude product and slurries point
From separating pressure 3Mpa, separation temperature is 40 DEG C；Remaining slurries use supercritical CO again2Extraction, in CO2It is added in fluid
Acetone, sldium lauryl sulfate, the acetone, sldium lauryl sulfate total dosage be CO2The 18% of fluid, wherein acetone, laruyl alcohol
The weight proportion of sodium sulphate is 1：0.5, control extracting pressure is 22MPa, and extraction temperature is 52 DEG C, CO2Flow is 22L/h, extraction
It is 1.3h to take the time, obtains tea polyphenols crude product b, tea polyphenols crude product is detached with slurries, separating pressure 5Mpa, separation temperature is
43 DEG C, gained tea polyphenols crude product a and tea polyphenols crude product b are mixed, addition hydrochloric acid, a concentration of the 22% of the hydrochloric acid, dosage is tea
The 13% of polyphenol crude product total amount, it is 3.3 to adjust pH value, centrifuges or is separated by filtration, obtains millet paste；
S4：Blade diameter length ratio by LX-8 types large pore resin absorption column on millet paste, LX-8 type large pore resin absorption columns is 1:6, applied sample amount
It it is 40 times of column volume, loading flow velocity is 0.8BV/h, first uses the ethanol aqueous wash removing that volume fraction is 1.5% miscellaneous, uses
Amount is 22 times, flow velocity 2BV/h of column volume, then the ethanol water for being 60% with volume fraction elutes, and dosage is column volume
13 times, flow velocity be 2 BV/h, collected volume score be 60% ethanol water eluent, be concentrated under reduced pressure, spray drying or
Tea polyphenols product is made in freeze-drying.
Embodiment 3
A kind of technique being isolated and purified tea polyphenols using tea grounds, is included the following steps：
S1：Tea grounds is dried and is ground into 200 mesh, then adds distilled water, be placed in vacuum high shear homogenizer fully it is homogeneous, obtain
To water pasty slurry, heating water bath is then used, makes the control of water pasty slurry temperature at 65 DEG C, and added in water pasty slurry
Ethyl alcohol stirs 10min with the speed of 500r/min, and slurries, the amount ratio of the tea grounds and distilled water are obtained after placing cooling 0.9h
It is 1:10-15, a concentration of the 37% of the ethyl alcohol, the amount ratio of tea grounds and ethyl alcohol is 1:0.6；
S2：Ultrasonication is carried out to slurries, the frequency of the ultrasonic wave is 30KHz, processing time 5min, and processing is made
Slurries；
S3：The slurries handled through step S2 are used into supercritical CO2Extraction, in CO2Sldium lauryl sulfate, acetic acid are added in fluid
Ethyl ester, polysorbate, the sldium lauryl sulfate, ethyl acetate, polysorbate total dosage be CO2The 22% of fluid, the wherein moon
Lauryl sulfate, ethyl acetate, polysorbate weight proportion be 2.5:1.5:2.6, control extracting pressure is 30MPa, extraction
Temperature is 52 DEG C, CO2Flow is 21L/h, extraction time 2h, obtains tea polyphenols crude product a, by tea polyphenols crude product and slurries point
From separating pressure 3.5Mpa, separation temperature is 42 DEG C；Remaining slurries use supercritical CO again2Extraction, in CO2Add in fluid
Enter acetone, sldium lauryl sulfate, the acetone, sldium lauryl sulfate total dosage be CO2The 18% of fluid, wherein acetone, bay
The weight proportion of alcohol sodium sulphate is 1：0.4, control extracting pressure is 22MPa, and extraction temperature is 52 DEG C, CO2Flow is 25L/h,
Extraction time is 1h, obtains tea polyphenols crude product b, tea polyphenols crude product is detached with slurries, separating pressure 3Mpa, and separation temperature is
40 DEG C, gained tea polyphenols crude product a and tea polyphenols crude product b are mixed, addition hydrochloric acid, a concentration of the 28% of the hydrochloric acid, dosage is tea
The 6% of polyphenol crude product total amount, it is 5.2 to adjust pH value, centrifuges or is separated by filtration, obtains millet paste；
S4：Blade diameter length ratio by LX-8 types large pore resin absorption column on millet paste, LX-8 type large pore resin absorption columns is 1:15, applied sample amount
It it is 56 times of column volume, loading flow velocity is 2 BV/h, and the ethanol aqueous wash that volume fraction is 7.5% is first used to remove miscellaneous, dosage
For 26 times of column volume, flow velocity be 4 BV/h, then the ethanol water for being 73% with volume fraction elutes, and dosage is column volume
18 times, flow velocity be 4 BV/h, collected volume score be 70% ethanol water eluent, be concentrated under reduced pressure, spray drying or
Tea polyphenols product is made in freeze-drying.
Comparative example 1
Preparation process is substantially the same manner as Example 1, has only the difference is that lacking in step S1 and adds ethyl alcohol in water pasty slurry,
The operating procedure of 10mi is stirred with the speed of 500r/min；Lack in CO in step S32CO is added in fluid2Fluid volume 15%
The operating procedure of sldium lauryl sulfate, ethyl acetate, polysorbate；Lack addition hydrochloric acid in step S3, it is 4.8 to adjust pH value
Operating procedure.
Comparative example 2
Preparation process is substantially the same manner as Example 1, has only the difference is that lacking in step S1 and adds ethyl alcohol in water pasty slurry,
The operating procedure of 10mi is stirred with the speed of 500r/min.
Comparative example 3
Preparation process is substantially the same manner as Example 1, has only the difference is that lacking in step s3 in CO2CO is added in fluid2Stream
The sldium lauryl sulfate of body dosage 15%, the operating procedure of ethyl acetate, polysorbate.
Comparative example 4
Preparation process is substantially the same manner as Example 1, has only the difference is that lacking addition hydrochloric acid in step s3, adjusting pH value is
4.8 operating procedure.
According to the tea polyphenols in technique extraction tea grounds described in embodiment 1-3 and comparative example 1-4, every group of experimental example takes 5kg tea
Slag, is detected tea polyphenol extract rate and purity, as a result see the table below shown：
| Experimental project | Recovery rate（%） | Purity（%） |
| Embodiment 1 | 16.78 | 99.68 |
| Embodiment 2 | 15.96 | 99.32 |
| Embodiment 3 | 16.51 | 99.54 |
| Comparative example 1 | 9.24 | 96.98 |
| Comparative example 2 | 15.21 | 99.09 |
| Comparative example 3 | 14.73 | 98.91 |
| Comparative example 4 | 14.95 | 98.97 |
As seen from the above table：（1）By the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment, tea polyphenol extract rate is obtained
With purity highest.
（2）By embodiment 2 and the data of comparative example 1-4 as it can be seen that step S1 adds ethyl alcohol in water pasty slurry, with
The operating procedure of the speed stirring 10mi of 500r/min；Lack in CO in step S32CO is added in fluid2The moon of fluid volume 15%
The operating procedure of lauryl sulfate, ethyl acetate, polysorbate；Lack addition hydrochloric acid in step S3, adjusts the behaviour that pH value is 4.8
Make step, synergistic effect is played during extracting tea polyphenols, collaboration improves the recovery rate and purity of tea polyphenols；This
It is：
Ethyl alcohol is added in step S1 in water pasty slurry, the ethyl alcohol of addition is polar solvent, and tea polyphenols are also polar substances, root
According to the principle of similar compatibility, ethyl alcohol can promote the dissolution of tea polyphenols in water, the dissolution without influencing other apolar substances
Rate；Heating water bath and 10mi is stirred with the speed of 500r/min simultaneously so that tea grounds internal temperature increases, and stirring can accelerate tea more
The diffusion of the extracts such as phenol, and then tea polyphenols is made quickly to be leached out, to increase the recovery rate and purity of tea polyphenols.Due to tea
Polyphenol is in CO2Solubility in fluid is little, causes its recovery rate not high, and the present invention lives according to sldium lauryl sulfate with surface
Change performance, solution can be made fully to activate, the characteristics of tea polyphenols are soluble in ethyl acetate and polysorbate can be as solubilizer
Micelle is formed in water, Adsorption of Tea Polyphenols substance and increase tea polyphenols in CO2The features such as solubility in fluid, in step s3 to
CO2CO is added in fluid2Sldium lauryl sulfate, ethyl acetate, the polysorbate of fluid volume 15%, it is possible to increase tea polyphenols are in CO2
Solubility in fluid；On the basis of adding ethyl alcohol into water pasty slurry in step sl, have in conjunction with sldium lauryl sulfate
Surfactant property can be such that solution fully activates and the characteristics of tea polyphenols are soluble in ethyl acetate, further increase tea polyphenols
Recovery rate.Tea polyphenols are stablized in acid condition, oxidizable under alkaline condition, and step S3 adds after tea polyphenol extract separation
Add acetic acid, it is 4.8 to adjust pH value, can prevent tea polyphenols from being aoxidized, to improve the purity of tea polyphenols.
The above content is it cannot be assumed that present invention specific implementation is confined to these explanations, for the technical field of the invention
Those of ordinary skill for, under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all answers
When being considered as belonging to present invention scope of patent protection determined by the appended claims.
Claims (10)
1. the technique for isolating and purifying tea polyphenols using tea grounds, which is characterized in that include the following steps：
S1, tea grounds feedstock processing；
S2, ultrasonication；
S3, supercritical CO2Extraction；
S4, it isolates and purifies；
The tea grounds feedstock processing, includes the following steps：
Tea grounds is dried and is ground into 120-200 mesh, then adds distilled water, be placed in vacuum high shear homogenizer fully it is homogeneous,
Water pasty slurry is obtained, heating water bath is then used, makes the control of water pasty slurry temperature at 60-65 DEG C, and in water pasty slurry
Middle addition ethyl alcohol stirs 10-25min with the speed of 200-500r/min, and slurries, the tea grounds are obtained after placing cooling 0.4-0.9h
Amount ratio with distilled water is 1:The amount ratio of 10-15, a concentration of 34%-38% of the ethyl alcohol, tea grounds and ethyl alcohol is 1:0.5-
0.8。
2. the technique according to claim 1 for isolating and purifying tea polyphenols using tea grounds, which is characterized in that described in step S2
Ultrasonication is to carry out ultrasonication to slurries, the slurries of processing is made, the frequency of the ultrasonic wave is 25-30KHz, place
The reason time is 5-8min.
3. the technique according to claim 1 for isolating and purifying tea polyphenols using tea grounds, which is characterized in that described in step S3
Supercritical CO2Extraction, includes the following steps：
The slurries handled through step S2 are used into supercritical CO2Extraction, in CO2Sldium lauryl sulfate, acetic acid second are added in fluid
Ester, polysorbate, control extracting pressure are 26-30MPa, and extraction temperature is 52-58 DEG C, CO2Flow is 20-25L/h, when extraction
Between be 1.5-3.5h, obtain tea polyphenols crude product a, tea polyphenols crude product detached with slurries, separating pressure 3-6Mpa, separation temperature
It is 40-50 DEG C；Remaining slurries use supercritical CO again2Extraction, in CO2Acetone, sldium lauryl sulfate, control are added in fluid
Extracting pressure is 22-27MPa, and extraction temperature is 50-56 DEG C, CO2Flow is 20-25L/h, and extraction time 1-2h obtains tea
Polyphenol crude product b detaches tea polyphenols crude product with slurries, separating pressure 3-6Mpa, and separation temperature is 40-50 DEG C, by gained tea
Polyphenol crude product a and the b mixing of tea polyphenols crude product, add hydrochloric acid, adjusting pH value is 3-5.2, centrifuges or is separated by filtration, obtains millet paste.
4. the technique according to claim 3 for isolating and purifying tea polyphenols using tea grounds, which is characterized in that the laruyl alcohol sulphur
Sour sodium, ethyl acetate, polysorbate total dosage be CO2The 15%-24% of fluid, wherein sldium lauryl sulfate, ethyl acetate, gather
The weight proportion of sorb ester is（1.2-2.5）:（0.6-2）:（1.5-3）.
5. the technique according to claim 4 for isolating and purifying tea polyphenols using tea grounds, which is characterized in that the laruyl alcohol sulphur
Sour sodium, ethyl acetate, polysorbate weight proportion be 1.8:2:2.6.
6. the technique according to claim 3 for isolating and purifying tea polyphenols using tea grounds, which is characterized in that the acetone, the moon
Total dosage of lauryl sulfate is CO2The 12%-18% of fluid, wherein acetone, sldium lauryl sulfate weight proportion be（1-2）：
（0.4-0.9）.
7. the technique according to claim 6 for isolating and purifying tea polyphenols using tea grounds, which is characterized in that the acetone, the moon
The weight proportion of lauryl sulfate is 1.6:0.8.
8. the technique according to claim 3 for isolating and purifying tea polyphenols using tea grounds, which is characterized in that the hydrochloric acid it is dense
Degree is 18%-28%, and dosage is the 6%-16% of tea polyphenols crude product total amount.
9. the technique according to claim 1 for isolating and purifying tea polyphenols using tea grounds, which is characterized in that described in step S4
It isolates and purifies, includes the following steps：
Blade diameter length ratio by LX-8 types large pore resin absorption column on millet paste, LX-8 type large pore resin absorption columns is 1:5-15, applied sample amount
It it is 37-56 times of column volume, loading flow velocity is 0 .5-2 BV/h, the ethanol aqueous wash for being first 1.2-7.5% with volume fraction
Remove miscellaneous, dosage is 20-26 times of column volume, flow velocity is 1-4 BV/h, then with volume fraction be 56%-73% ethyl alcohol it is water-soluble
Liquid elutes, and dosage is 12-18 times of column volume, flow velocity is 1-4 BV/h, and collected volume score is that the ethyl alcohol of 56%-73% is water-soluble
The eluent of liquid is concentrated under reduced pressure, and spray drying is dry, and tea polyphenols product is made.
10. the technique according to claim 9 for isolating and purifying tea polyphenols using tea grounds, which is characterized in that institute in step S4
It is spray drying or freeze-drying to state dry.
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| CN1683363A (en) * | 2005-03-11 | 2005-10-19 | 中山大学 | Method for extracting catechin from tea |
| CN103704421A (en) * | 2013-12-13 | 2014-04-09 | 福州市东苹企业管理服务有限公司 | Ultrasonic supercritical combined extraction technology for tea polyphenol |
| CN104398669A (en) * | 2014-10-31 | 2015-03-11 | 陕西师范大学 | Caffeine-free tea polyphenol separation purification method |
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|---|---|---|---|---|
| CN1683363A (en) * | 2005-03-11 | 2005-10-19 | 中山大学 | Method for extracting catechin from tea |
| CN103704421A (en) * | 2013-12-13 | 2014-04-09 | 福州市东苹企业管理服务有限公司 | Ultrasonic supercritical combined extraction technology for tea polyphenol |
| CN104398669A (en) * | 2014-10-31 | 2015-03-11 | 陕西师范大学 | Caffeine-free tea polyphenol separation purification method |
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Application publication date: 20181009 |