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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 PDF

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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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black tea
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CN107320576B (en
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管天球
管敏
管晖
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/82Theaceae (Tea family), e.g. camellia
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/105Plant extracts, their artificial duplicates or their derivatives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/17Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Food Science & Technology (AREA)
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  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Medicines Containing Plant Substances (AREA)
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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

A kind of extracting method of black tea golden flower nutritional ingredients
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.
CN201710503031.2A 2017-06-27 2017-06-27 Method for extracting nutritional ingredients of dark tea golden flowers Expired - Fee Related CN107320576B (en)

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CN108450567A (en) * 2018-04-20 2018-08-28 管天球 A kind of preparation method of preventing hypertension tea oil
CN111955572A (en) * 2020-06-09 2020-11-20 江苏华桑食品科技有限公司 Method for extracting concentrated tea liquid

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CN103739735A (en) * 2014-01-23 2014-04-23 李文东 Method for extracting tea polysaccharide from dark tea eurotium cristatum
CN104738252A (en) * 2015-03-07 2015-07-01 西安康坊食品有限公司 Method for preparing instant tea from fu brick tea
CN106188323A (en) * 2016-07-07 2016-12-07 南京农业大学 A kind of method preparing the Fu-brick tea tea polysaccharide with the prebiotic function of intestinal

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108450567A (en) * 2018-04-20 2018-08-28 管天球 A kind of preparation method of preventing hypertension tea oil
CN111955572A (en) * 2020-06-09 2020-11-20 江苏华桑食品科技有限公司 Method for extracting concentrated tea liquid

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