CN107320576A - A kind of extracting method of black tea golden flower nutritional ingredients - Google Patents
A kind of extracting method of black tea golden flower nutritional ingredients Download PDFInfo
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- CN107320576A CN107320576A CN201710503031.2A CN201710503031A CN107320576A CN 107320576 A CN107320576 A CN 107320576A CN 201710503031 A CN201710503031 A CN 201710503031A CN 107320576 A CN107320576 A CN 107320576A
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- 244000269722 Thea sinensis Species 0.000 title claims abstract description 69
- 235000020279 black tea Nutrition 0.000 title claims abstract description 65
- 235000006468 Thea sinensis Nutrition 0.000 title claims abstract description 63
- 235000016709 nutrition Nutrition 0.000 title claims abstract description 29
- 239000004615 ingredient Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 63
- 238000001914 filtration Methods 0.000 claims abstract description 24
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 239000000284 extract Substances 0.000 claims description 27
- 239000007864 aqueous solution Substances 0.000 claims description 23
- 239000011347 resin Substances 0.000 claims description 17
- 229920005989 resin Polymers 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 16
- 239000002250 absorbent Substances 0.000 claims description 14
- 230000002745 absorbent Effects 0.000 claims description 14
- 238000002386 leaching Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000000243 solution Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 6
- 239000003480 eluent Substances 0.000 claims description 6
- 239000011552 falling film Substances 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 235000013616 tea Nutrition 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000001488 sodium phosphate Substances 0.000 claims description 4
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- 239000011260 aqueous acid Substances 0.000 claims description 3
- 239000011449 brick Substances 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000000108 ultra-filtration Methods 0.000 claims description 3
- 235000005979 Citrus limon Nutrition 0.000 claims description 2
- 244000131522 Citrus pyriformis Species 0.000 claims description 2
- 239000003463 adsorbent Substances 0.000 claims description 2
- 239000001273 butane Substances 0.000 claims description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 2
- 239000002689 soil Substances 0.000 claims 1
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 235000013305 food Nutrition 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 description 5
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000035764 nutrition Effects 0.000 description 3
- 206010021143 Hypoxia Diseases 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
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 229960001948 caffeine Drugs 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
- 230000009514 concussion Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 230000007954 hypoxia Effects 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 239000002075 main ingredient Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000003053 toxin Substances 0.000 description 2
- 231100000765 toxin Toxicity 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 235000013406 prebiotics Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- COEZWFYORILMOM-UHFFFAOYSA-N sodium 4-[(2,4-dihydroxyphenyl)diazenyl]benzenesulfonic acid Chemical compound [Na+].OC1=CC(O)=CC=C1N=NC1=CC=C(S(O)(=O)=O)C=C1 COEZWFYORILMOM-UHFFFAOYSA-N 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Classifications
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- 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 OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- 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
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- 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
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- 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
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Tea And Coffee (AREA)
Abstract
A kind of extracting method of black tea golden flower nutritional ingredients disclosed by the invention, is related to biomedicine technical field, its technological process is as follows:(1), crush;(2), flooding;(3), alcohol steep;(4), just concentration;(5), just merge;(6), pH value is adjusted;(7), filter;(8), adsorb;(9), elute;(10), it is combined simultaneously;(11), multiple concentration;(12), removal of impurities;(13), refined filtration;(14), dry.The features such as with black tea golden flower nutritional ingredients effectively can be extracted from black tea, nourishing additive agent of its product mainly as various food;The extracting method of the black tea golden flower nutritional ingredients of the present invention, it is adaptable to black tea golden flower nutritional ingredients are extracted from various black teas.
Description
Technical field
The present invention relates to biomedicine technical field, particularly a kind of extracting method of black tea golden flower nutritional ingredients.
Background technology
Black tea belongs to full fermentation tea, and it produces a kind of unique golden yellow coloured particles in process, is found through scientific research, the gold
Yellow particle is a kind of prebiotic thalline being highly profitable to human body, and expert is named as " coronoid process dissipate capsule bacterium ", is commonly called as " black tea golden flower ".
Because " product that black tea golden flower " is produced with reducing fat, reduce blood fat, toxin expelling defaecation, warm stomach invigorating the spleen, promotes digestion, clearly
The plurality of health care functions such as enteron aisle are managed, thus, black tea golden flower nutritional ingredient has liver protecting, pre- preventing tumor, removes toxin, increases
Strong cell hypoxia-bearing capability, whole body fatigue is eliminated, human body hypoxia-bearing capability, the conveying for promoting blood oxygen and cell can be improved utilizes
Deng healthcare function, the health demand of sub-health population can be effectively solved.
At present, the extraction of black tea golden flower nutritional ingredients or preparation method, there is not been reported.
Chinese patent (number of patent application is 2014100319322) is disclosed, and " one kind extracts tea polysaccharide from black tea golden flower
Method ", including raw material is crushed, concussion for the first time is extracted, second concussion is extracted, once concentration, precipitation, upper prop, secondary dense
Contracting, drying and other steps;For extracting tea polysaccharide from black tea golden flower.
The content of the invention
The technical problems to be solved by the invention are to provide one kind can effectively extract black tea golden flower nutrition from black tea
The method of composition.
The technical solution used in the present invention is to invent a kind of extracting method of black tea golden flower nutritional ingredients, its technological process
It is as follows:
(1), crush:Black tea is first processed into coarse fodders more than 20 mesh, is then transferred in baking oven, is dried at 35-40 DEG C
It is less than 8% to moisture, obtains black tea coarse fodder, it is standby;
(2), flooding:Black tea coarse fodder is placed in extractor, is added into extractor and accounts for the clear of former 5~6 times of black tea weight
Water, in the case where temperature is 38~50 DEG C, extracting at constant temperature 1~2 hour, filtering, obtain water extract, standby;
(3), alcohol steep:The second for accounting for that former 6~8 times of black tea weight, volumetric concentration are 50-70% is added into extractor again
Alcohol, the extracting at constant temperature 50-80min in the case where temperature is 40-65 DEG C, filtering obtains first time alcohol extract;Added again into extractor
The ethanol of former times of amount, extracts 20-42min at the same temperature, filters, obtains second of alcohol extract;First time ethanol is soaked
Extract and second of alcohol extract merge, and obtain the total leaching liquor of ethanol, standby;
(4), just concentration:The total leaching liquor of ethanol is transferred in falling film condenser, temperature be 50-58 DEG C, pressure be 12-
No alcohol is concentrated under 19KPa, filters, obtains concentration leaching liquor, it is standby;
(5), just merge:Water extract is merged with concentration leaching liquor, stirred evenly, black tea is obtained and mixes extract, it is standby;
(6), pH value is adjusted:Mixed to black tea and the weak base aqueous solution that weight concentration is 0.1-1.2% is added in extract, adjust pH
It is worth for 9-11, stirs evenly, obtains pH value regulation liquid, it is standby;
(7), filter:PH value regulation liquid is transferred in freezer, quiet in the case where temperature is 4-10 DEG C to put 5-8h, filtering was collected
Filtrate is standby;
(8), adsorb:Filtered fluid is heated to 40-46 DEG C by 1-3 DEG C/min heating rate, then upper low pole macropore is inhaled
Attached resin (such as AB-8, D101, HPD-400), upper prop liquid measure is 2-2.5 times of low pole macroporous absorbent resin weight, flow velocity
For 0.5-0.8L/10min, upper prop liquid is collected, it is standby;
(9), elute:Low pole is eluted with the sodium hydroxide solution that weight concentration is 0.15-0.35%, temperature is 8-15 DEG C
Macroporous absorbent resin, consumption is 1-1.5 times of low pole macroporous absorbent resin weight, and flow velocity is 3-5L/h;Weight concentration is used again
Low pole macroporous absorbent resin is eluted at normal temperatures for 0.5-1.8% aqueous acid, and consumption is low pole macroporous absorbent resin
2.5-4.0 times of weight, flow velocity is 3-5L/h;Then the ethanol solution for being 65-80% with volumetric concentration elutes low pole macropore
Polymeric adsorbent, consumption is 2.0-2.5 times of column volume, and flow velocity is 1.5-2.0L/10min, collects the ethanol eluate of this section, standby
With;
(10), it is combined simultaneously:Upper prop liquid and ethanol eluate are merged, eluent mixture is obtained, it is standby;
(11), multiple concentration:Eluent mixture is transferred in falling film condenser, temperature be 60-75 DEG C, pressure be 8-
Solid content is concentrated under 15KPa for 0.65-1.2mg/10ml, concentrate is obtained, it is standby;
(12), removal of impurities:The organic solvent of 5-6 times of weight is added into concentrate, 10- is stirred in the case where temperature is 35-45 DEG C
18min, stands, is layered, filters, collect the aqueous solution of lower floor;Then added again into the aqueous solution and account for aqueous solution weight 5-8%'s
Emathlite, the stir process 20-28min in the case where temperature is 60-75 DEG C, filtering obtains the processing aqueous solution, standby;
(13), refined filtration:The aqueous solution ultra-filtration membrane device that via hole diameter is 10-20nm in the case where pressure is 0.2-0.35MPa will be handled
Filtering, collects filtering aqueous, standby;
(14), dry:Aqueous will be filtered spray-dried, and produce black tea golden flower nutritional ingredients.
Described black tea is weight shared by black tea golden flower than the black tea Fu-brick tea more than 5%.
Described weak base aqueous solution is the aqueous solution of sodium acid carbonate or sodium phosphate or dibastic sodium phosphate.
Described sour water is the aqueous solution of citric acid or watery hydrochloric acid or oxalic acid.
Described organic solvent is one kind in n-hexane, No. six solvent naphthas, butane.
The extracting method of the black tea golden flower nutritional ingredients of the present invention, is carried by the way of flooding and alcohol extraction develop simultaneously
Take, black tea golden flower nutritional ingredient is not only extracted to greatest extent but also the caffeine in tealeaves, heavy metal, color is greatly reduced
Element etc. is harmful or hinders the extraction of material.Meanwhile, by absorption and three elutions, effectively further isolate in extraction solution
The materials such as the caffeine, pigment, the glycoside that are remained in the material such as free heavy metal or suspension and solution, then take milipore filter
Device is filtered so that the impurity such as excessive pigment of molecular weight is further removed, so as to ensure that product quality and nutrition
The enrichment of composition.It ensure that the high content of black tea golden flower nutritional ingredients in extraction of substance.
Embodiment
With reference to embodiments, the present invention is described further.Following explanation is but this hair in the way of enumerating
Bright protection domain is not limited thereto.
The extracting method of the black tea golden flower nutritional ingredients of the present embodiment, its technological process is as follows:
(1), crush:First the weight shared by black tea golden flower is processed into more than 20 mesh than the black tea Fu-brick tea more than 5%
Coarse fodder, is then transferred in baking oven, is dried at 38 DEG C to moisture and is less than 8%, obtains black tea coarse fodder, standby;
(2), flooding:Black tea coarse fodder is placed in extractor, is added into extractor and accounts for the clear of former 5.5 times of black tea weight
Water, in the case where temperature is 45 DEG C, extracting at constant temperature 1.5 hours, filtering, obtain water extract, standby;
(3), alcohol steep:The ethanol for accounting for that former 7 times of black tea weight, volumetric concentration are 60% is added into extractor again, in temperature
Spend for extracting at constant temperature 65min at 55 DEG C, filtering obtains first time alcohol extract;The ethanol of former times of amount is added into extractor again,
30min is extracted at the same temperature, is filtered, is obtained second of alcohol extract;By first time alcohol extract and second of ethanol
Leaching liquor merges, and obtains the total leaching liquor of ethanol, standby;
(4), just concentration:The total leaching liquor of ethanol is transferred in falling film condenser, is 55 DEG C, under pressure is 15KPa in temperature
No alcohol is concentrated into, filters, obtains concentration leaching liquor, it is standby;
(5), just merge:Water extract is merged with concentration leaching liquor, stirred evenly, black tea is obtained and mixes extract, it is standby;
(6), pH value is adjusted:Mixed to black tea and the sodium bicarbonate aqueous solution that weight concentration is 0.8% is added in extract, adjust pH
It is worth for 10, stirs evenly, obtains pH value regulation liquid, it is standby;
(7), filter:PH value regulation liquid is transferred in freezer, quiet in the case where temperature is 6 DEG C to put 6h, filtered fluid is collected in filtering,
It is standby;
(8), adsorb:Filtered fluid is heated to 45 DEG C by 2 DEG C/min heating rate, then, upper low pole macroporous absorption tree
Fat (this example uses HPD-400), upper prop liquid measure is 2.2 times of low pole macroporous absorbent resin weight, and flow velocity is 0.6L/10min,
Upper prop liquid is collected, it is standby;
(9), elute:It is that the sodium hydroxide solution that 0.25%, temperature is 12 DEG C elutes low pole macroporous absorption with weight concentration
Resin, consumption is 1.2 times of low pole macroporous absorbent resin weight, and flow velocity is 4L/h;Again with the lemon that weight concentration is 1.2%
Aqueous acid elutes low pole macroporous absorbent resin at normal temperatures, and consumption is 3.5 times of low pole macroporous absorbent resin weight, stream
Speed is 4L/h;Then it is 70% ethanol solution elution low pole macroporous absorbent resin with volumetric concentration, consumption is 2.2 times of post
Volume, flow velocity is 1.8L/10min, collects the ethanol eluate of this section, standby;
(10), it is combined simultaneously:Upper prop liquid and ethanol eluate are merged, eluent mixture is obtained, it is standby;
(11), multiple concentration:Eluent mixture is transferred in falling film condenser, temperature be 65 DEG C, pressure be under 12KPa it is dense
Solid content is reduced to for 0.8mg/10ml, concentrate is obtained, it is standby;
(12), removal of impurities:The n-hexane of 5.5 times of weight is added into concentrate, 15min is stirred in the case where temperature is 40 DEG C, stand,
Layering, filtering, collect the aqueous solution of lower floor;Then the Emathlite for accounting for aqueous solution weight 6% is added into the aqueous solution again, in temperature
Spend for stir process 25min at 65 DEG C, filtering obtains the processing aqueous solution, standby;
(13), refined filtration:By the processing aqueous solution ultra-filtration membrane device that via hole diameter is 15nm in the case where pressure is 0.3MPa filtering, collect
Aqueous is filtered, it is standby;
(14), dry:Aqueous will be filtered spray-dried, and produce black tea golden flower nutritional ingredients.
Following table 1 is the Main Ingredients and Appearance content detection data for the black tea golden flower nutritional ingredients that the present embodiment is extracted.
Main Ingredients and Appearance content detection table in the black tea golden flower nutritional ingredients of table 1
The black tea golden flower nutritional ingredients that the present invention is extracted, mainly as the nourishing additive agent of various food.
The extracting method of the black tea golden flower nutritional ingredients of the present invention, it is adaptable to black tea golden flower nutrition is extracted from various black teas
Composition.
Claims (5)
1. a kind of extracting method of black tea golden flower nutritional ingredients, it is characterised in that technological process is as follows:
(1), crush:Black tea is first processed into coarse fodders more than 20 mesh, is then transferred in baking oven, is dried at 35-40 DEG C to water
Divide and be less than 8%, obtain black tea coarse fodder, it is standby;
(2), flooding:Black tea coarse fodder is placed in extractor, the clear water for accounting for former 5~6 times of black tea weight is added into extractor,
In the case where temperature is 38~50 DEG C, extracting at constant temperature 1~2 hour, filtering, obtain water extract, standby;
(3), alcohol steep:The ethanol for accounting for that former 6~8 times of black tea weight, volumetric concentration are 50-70% is added into extractor again,
Temperature is extracting at constant temperature 50-80min at 40-65 DEG C, and filtering obtains first time alcohol extract;Former times is added into extractor again
The ethanol of amount, extracts 20-42min at the same temperature, filtering, obtains second of alcohol extract;By first time alcohol extract
Merge with second of alcohol extract, obtain the total leaching liquor of ethanol, it is standby;
(4), just concentration:The total leaching liquor of ethanol is transferred in falling film condenser, temperature be 50-58 DEG C, pressure be 12-19KPa
Under be concentrated into no alcohol, filter, obtain concentration leaching liquor, it is standby;
(5), just merge:Water extract is merged with concentration leaching liquor, stirred evenly, black tea is obtained and mixes extract, it is standby;
(6), pH value is adjusted:Mixed to black tea and the weak base aqueous solution that weight concentration is 0.1-1.2% is added in extract, regulation pH value is
9-11, is stirred evenly, and obtains pH value regulation liquid, standby;
(7), filter:PH value regulation liquid is transferred in freezer, quiet in the case where temperature is 4-10 DEG C to put 5-8h, filtering is collected in filtering
Liquid, it is standby;
(8), adsorb:Filtered fluid is heated to 40-46 DEG C by 1-3 DEG C/min heating rate, then upper low pole macroporous absorption tree
Fat, upper prop liquid measure is 2-2.5 times of low pole macroporous absorbent resin weight, and flow velocity is 0.5-0.8L/10min, collects upper prop liquid,
It is standby;
(9), elute:Low pole macropore is eluted with the sodium hydroxide solution that weight concentration is 0.15-0.35%, temperature is 8-15 DEG C
Polymeric adsorbent, consumption is 1-1.5 times of low pole macroporous absorbent resin weight, and flow velocity is 3-5L/h;It is with weight concentration again
0.5-1.8% aqueous acid elutes low pole macroporous absorbent resin at normal temperatures, and consumption is low pole macroporous absorbent resin weight
2.5-4.0 times of amount, flow velocity is 3-5L/h;Then the ethanol solution for being 65-80% with volumetric concentration elution low pole macropore is inhaled
Attached resin, consumption is 2.0-2.5 times of column volume, and flow velocity is 1.5-2.0L/10min, collects the ethanol eluate of this section, standby
With;
(10), it is combined simultaneously:Upper prop liquid and ethanol eluate are merged, eluent mixture is obtained, it is standby;
(11), multiple concentration:Eluent mixture is transferred in falling film condenser, is 60-75 DEG C, under pressure is 8-15KPa in temperature
Solid content is concentrated into for 0.65-1.2mg/10ml, concentrate is obtained, it is standby;
(12), removal of impurities:The organic solvent of 5-6 times of weight is added into concentrate, 10-18min is stirred in the case where temperature is 35-45 DEG C,
Stand, be layered, filter, collect the aqueous solution of lower floor;Then added again into the aqueous solution and account for the acid white of aqueous solution weight 5-8%
Soil, the stir process 20-28min in the case where temperature is 60-75 DEG C, filtering obtains the processing aqueous solution, standby;
(13), refined filtration:By the processing aqueous solution ultra-filtration membrane device that via hole diameter is 10-20nm in the case where pressure is 0.2-0.35MPa filtering,
Filtering aqueous is collected, it is standby;
(14), dry:Aqueous will be filtered spray-dried, and produce black tea golden flower nutritional ingredients.
2. the extracting method of black tea golden flower nutritional ingredients according to claim 1, it is characterised in that:Described black tea is black tea
Weight shared by golden flower is than the black tea Fu-brick tea more than 5%.
3. the extracting method of black tea golden flower nutritional ingredients according to claim 1 or claim 2, it is characterised in that:Described week-base water
Solution is the aqueous solution of sodium acid carbonate or sodium phosphate or dibastic sodium phosphate.
4. the extracting method of black tea golden flower nutritional ingredients according to claim 3, it is characterised in that:Described sour water is lemon
The aqueous solution of acid or watery hydrochloric acid or oxalic acid.
5. the extracting method of black tea golden flower nutritional ingredients according to claim 4, it is characterised in that:Described organic solvent is
One kind in n-hexane, No. six solvent naphthas, butane.
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