CN109320629A - A kind of extracting method of tea polysaccharide - Google Patents

A kind of extracting method of tea polysaccharide Download PDF

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Publication number
CN109320629A
CN109320629A CN201811527785.2A CN201811527785A CN109320629A CN 109320629 A CN109320629 A CN 109320629A CN 201811527785 A CN201811527785 A CN 201811527785A CN 109320629 A CN109320629 A CN 109320629A
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China
Prior art keywords
iron
tea polysaccharide
dried
extracting method
ethyl acetate
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CN201811527785.2A
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Chinese (zh)
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椤惧嘲
顾峰
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CHENGDU WAGOTT BIO-TECH Co Ltd
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CHENGDU WAGOTT BIO-TECH Co Ltd
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Priority to CN201811527785.2A priority Critical patent/CN109320629A/en
Publication of CN109320629A publication Critical patent/CN109320629A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Molecular Biology (AREA)
  • General Health & Medical Sciences (AREA)
  • Sustainable Development (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The present invention discloses a kind of extracting method of tea polysaccharide, belongs to deep processing field of tea comprising the steps of: S1 is extracted: being carried out soak extraction to tealeaves with purified water and is obtained leaching liquor;S2 abstraction impurity removal: ethyl acetate is added in the leaching liquor and carries out abstraction impurity removal, collects water phase;S3 concentration and recovery: by water phase obtained by S2 carry out recycling catch up with it is molten;S4 filtering: S3 obtained aqueous solution is crossed into film, cleaner liquid is obtained by filtration;S5 be concentrated and dried: by the cleaner liquid be concentrated into solid content be 40% after, be spray-dried;S6 pulverizes and sieves except iron: will be spray-dried obtained solid and is crushed with pulverizer, cross mesh, remove iron with magnet absorption, except powder is uniformly mixed after iron, qualified products are made after removing iron in sieving, magnet absorption again.This method uses tealeaves for raw material, directly carries out primary soak extraction with purified water, then and removal of impurities is extracted with ethyl acetate, overcome the disadvantages of yield in traditional handicraft is low, poor product quality, and dissolubility is unstable, improve the recovery rate of tea polysaccharide.

Description

A kind of extracting method of tea polysaccharide
Technical field
The invention belongs to deep processing field of tea, are related to a kind of extracting method of tea polysaccharide.
Background technique
Tea polysaccharide is a kind of complex polysaccharide with certain physiological activity, and real name should claim tea active polysaccharide, it is different from tea The substance polysaccharide such as cellulose, hemicellulose, starch in leaf.
Tea polysaccharide is a kind of acidoglycoprotein, and is combined with a large amount of mineral element, referred to as Tea Polysaccharides compound, referred to as For Tea Polysaccharides or tea polysaccharide (TeaPolysaccharide).Wherein protein part is mainly by about 20 kinds of common amino acid groups At, sugared part mainly by arabinose, xylose, fucose, glucose, galactolipin etc., mineral element mainly by calcium, magnesium, iron, Manganese etc. and a small amount of microelement, such as rare earth element composition.
A kind of natural active matter of the tea polysaccharide as great exploitation potential, functional study are always researcher's concern Emphasis.Since Japanese scholars clear water Cen husband reports that tea polysaccharide has bioactive functions, a large amount of tea polysaccharide functional studies are real Verifying is real, and tea polysaccharide has following multiple biological activities: (1) hypoglycemic;(2) reducing blood lipid;(3) it adjusts immune;(4) anticoagulation, Antithrombotic;(5) anti-oxidant etc..Furthermore tea polysaccharide can also reducing heart rate, increase coronary flow and the effects of resist oxygen lack, in recent years It was found that tea polysaccharide also has effects that treat diabetes.
The method that current tea polysaccharide extracts mainly has water extract-alcohol precipitation extraction, ultrasonic wave extraction, Microwave Extraction, enzyme to extract Deng wherein water extract-alcohol precipitation extraction is also divided into that hot water alcohol precipitation extracts, cold water alcohol precipitation extracts, acidleach formulation and alkali method, hot water It is high that water alcohol precipitation extracts the recovery rate extracted relative to cold water alcohol precipitation, but the researchs such as Wang Dongfeng confirm, the thermal stability of tea polysaccharide is poor; Acidleach formulation and alkali method are easily destroyed the structure of polysaccharide, and tea polysaccharide is caused to lose;Ultrasonic wave extraction will lead to tea polysaccharide Activity reduce or inactivation;Microwave Extraction energy consumption is high and temperature is high;Enzyme extraction method causes extraction cost excessively high due to enzyme price height; The recovery rate of existing tea polysaccharide a maximum of about of 5%.
Summary of the invention
Recovery rate in order to solve the problems, such as above-mentioned tea polysaccharide of the existing technology is too low, and present invention offer one grows tea more The extracting method of sugar.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of extracting method of tea polysaccharide comprising the steps of:
S1 is extracted: purified water being added in tealeaves and is impregnated, leaching liquor is obtained;
S2 abstraction impurity removal: ethyl acetate is added in the leaching liquor and carries out abstraction impurity removal, collects water phase;
S3 concentration and recovery: by water phase obtained by S2 carry out recycling catch up with it is molten;
S4 filtering: S3 obtained aqueous solution is crossed into film, cleaner liquid is obtained by filtration;
S5 be concentrated and dried: by the cleaner liquid be concentrated into solid content be 40% after, be spray-dried;
S6 pulverizes and sieves except iron: spray drying obtained solid crushed with pulverizer, crosses 60-80 mesh, removes iron with magnet absorption, Except powder is uniformly mixed after iron, sieving, magnet absorption are except qualified products obtained after iron again.
Further, Extracting temperature is 65 DEG C -75 DEG C in S1.
Further, the additional amount of ethyl acetate described in S2 is 2 times of leaching liquor weight.
Further, filter sizes used are 0.2 μm in S4.
Further, the condition being spray-dried in S5 is to control 175-220 DEG C of inlet air temperature, 80-125 DEG C of leaving air temp.
Compared with prior art, the beneficial effects of the present invention are:
(1) this method uses tealeaves for raw material, directly carries out primary soak extraction with purified water, then and is extracted with ethyl acetate and removes It is miscellaneous, the disadvantages of yield in traditional handicraft is low, poor product quality, and dissolubility is unstable is overcome, the recovery rate of tea polysaccharide is improved;
(2) it uses film filtering membrane aperture for 0.2 μm of equipment in purifying process, the yield of tea polysaccharide is made to obtain biggish mention It is high;
(3) method have it is easy to operate, separative efficiency is high, at low cost, with short production cycle, the high advantage of the product purity of production, It is mass produced suitable for batch production.
Specific embodiment
The present invention will be further described with reference to the examples below, and described embodiment is only present invention a part Embodiment is not whole embodiment.Based on the embodiments of the present invention, those skilled in the art are not making Other all embodiments obtained, belong to protection scope of the present invention under the premise of creative work.
Embodiment 1:
Tealeaves is added in agitator tank, the purified water that volume is 5 times of tealeaves volume is added and carries out soak extraction 2h, soaking temperature is 65 DEG C, leaching liquor is entered into lower process;Leaching liquor is extracted with ethyl acetate, the additional amount of ethyl acetate is leaching liquor weight 2 times, sufficiently after extraction, collect water phase;Gained water phase is recycled, is warming up to 90 DEG C in water phase with outer circulation inspissator Ethyl acetate solvent is caught up with only;By catch up with it is molten after water phase cross film and be collected by filtration cleaner liquid, the membrane aperture of film used is 0.2 μm;It will filter Clear liquid is concentrated into after solid content is 40% and is spray-dried, and the condition of spray drying is 175 DEG C of inlet air temperature, leaving air temp 80 ℃;Spray drying obtained solid is crushed with pulverizer, crosses 70 meshes, removes iron with magnet absorption, it is equal except powder is mixed after iron Even, sieving, magnet absorption are except obtained after iron again.Yield is 20%, purity 42%.
Embodiment 2:
Tealeaves is added in agitator tank, the purified water that volume is 5 times of tealeaves volume is added and carries out soak extraction 2h, soaking temperature is 75 DEG C, leaching liquor is entered into lower process;Leaching liquor is extracted with ethyl acetate, the additional amount of ethyl acetate is leaching liquor weight 2 times, sufficiently after extraction, collect water phase;Gained water phase is recycled, is warming up to 90 DEG C in water phase with outer circulation inspissator Ethyl acetate solvent is caught up with only;By catch up with it is molten after water phase cross film and be collected by filtration cleaner liquid, the membrane aperture of film used is 0.2 μm;It will filter Clear liquid is concentrated into after solid content is 40% and is spray-dried, and the condition of spray drying is 220 DEG C of inlet air temperature, leaving air temp 125℃;Spray drying obtained solid is crushed with pulverizer, 80 meshes are crossed, removes iron with magnet absorption, except mixing powder after iron Uniformly, sieving, magnet absorption are made after removing iron again.Yield is 21%, purity 44%.
Embodiment 3:
Tealeaves is added in agitator tank, the purified water that volume is 5 times of tealeaves volume is added and carries out soak extraction 2h, soaking temperature is 70 DEG C, leaching liquor is entered into lower process;Leaching liquor is extracted with ethyl acetate, the additional amount of ethyl acetate is leaching liquor weight 2 times, sufficiently after extraction, collect water phase;Gained water phase is recycled, is warming up to 90 DEG C in water phase with outer circulation inspissator Ethyl acetate solvent is caught up with only;By catch up with it is molten after water phase cross film and be collected by filtration cleaner liquid, the membrane aperture of film used is 0.2 μm;It will filter Clear liquid is concentrated into after solid content is 40% and is spray-dried, and the condition of spray drying is 200 DEG C of inlet air temperature, leaving air temp 100℃;Spray drying obtained solid is crushed with pulverizer, 60 meshes are crossed, removes iron with magnet absorption, except mixing powder after iron Uniformly, sieving, magnet absorption are made after removing iron again.Yield is 20%, purity 40%.
Comparative example 1:
Tealeaves is added in agitator tank, the ethyl acetate that 3 times of equivalents are added impregnates 1-2h, and the soak in agitator tank is transferred to Lower process;Tea grounds after infusion of tea is dried with slag machine is dried, then purified water is added in the tea grounds of drying again and is extracted, is mentioned Temperature≤65 DEG C are taken, it is solid containing being sprayed that leaching liquor is concentrated into 40%;Spray drying obtained solid is crushed with pulverizer, mistake 60-90 mesh removes iron with magnet absorption, and except powder is uniformly mixed after iron, sieving, magnet absorption are except obtained after iron again.It receives Rate is 15%, purity 30%.
By embodiment 1 and comparative example 1 and as it can be seen that inventive concept of the invention is first to be extracted in tealeaves to own with purified water Water-soluble substances obtain leaching liquor, recycle this characteristic of tea polysaccharide insoluble in ethyl acetate, removed using ethyl acetate The impurity in leaching liquor is removed, target product tea polysaccharide is then dried to obtain by filtering and concentrating;Comparative example 1 also utilizes tea Polysaccharide does not dissolve in this characteristic of ethyl acetate, and still, comparative example 1 is first to extract in tealeaves to be dissolved in acetic acid using ethyl acetate The impurity of ethyl ester, then by the purified water soak extraction tea polysaccharide of the tea grounds after ethyl acetate impregnates, the yield of comparative example 1 and pure Degree is all not as good as embodiment 2.
Disclosed above is only presently preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly It encloses, therefore makees ground equivalent variations according to the claims in the present invention, be still within the scope of the present invention.

Claims (5)

1. a kind of extracting method of tea polysaccharide, which is characterized in that comprise the steps of:
S1 is extracted: purified water being added in tealeaves and is impregnated, leaching liquor is obtained;
S2 abstraction impurity removal: ethyl acetate is added in the leaching liquor and carries out abstraction impurity removal, collects water phase;
S3 concentration and recovery: by water phase obtained by S2 carry out recycling catch up with it is molten;
S4 filtering: S3 obtained aqueous solution is crossed into film, cleaner liquid is obtained by filtration;
S5 be concentrated and dried: by the cleaner liquid be concentrated into solid content be 40% after, be spray-dried;
S6 pulverizes and sieves except iron: spray drying obtained solid crushed with pulverizer, crosses 60-80 mesh, removes iron with magnet absorption, Except powder is uniformly mixed after iron, sieving, magnet absorption are except qualified products obtained after iron again.
2. a kind of extracting method of tea polysaccharide according to claim 1, which is characterized in that in S1 Extracting temperature be 65 DEG C- 75℃。
3. a kind of extracting method of tea polysaccharide according to claim 1, which is characterized in that ethyl acetate described in S2 adds Enter 2 times that amount is leaching liquor weight.
4. a kind of extracting method of tea polysaccharide according to claim 1, which is characterized in that filter sizes used are in S4 0.2μm。
5. a kind of extracting method of tea polysaccharide according to claim 1, which is characterized in that the condition being spray-dried in S5 To control 175-220 DEG C of inlet air temperature, 80-125 DEG C of leaving air temp.
CN201811527785.2A 2018-12-13 2018-12-13 A kind of extracting method of tea polysaccharide Pending CN109320629A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1431226A (en) * 2003-01-13 2003-07-23 浙江大学 Method for extracting tea polysaccharide from tailings with tea polyphenols being extracted
CN102060937A (en) * 2011-02-25 2011-05-18 余芳 Extraction and separation method for green tea polysaccharides
CN103819311A (en) * 2014-02-26 2014-05-28 成都华高生物制品有限公司 Method for extracting high-content tea polyphenol from fresh tea
CN104211824A (en) * 2014-08-27 2014-12-17 陕西盛迈石油有限公司 Preparation method of tea polysaccharide
CN105273103A (en) * 2015-11-12 2016-01-27 云南茶农生物产业有限责任公司 Method for preparing tea polysaccharides by combining separating membranes with chromatographic column
CN108440481A (en) * 2018-04-20 2018-08-24 佛山推启农业研究院(普通合伙) A kind of microwave combined method for extracting effective ingredient in thick tea of ultrasound-

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1431226A (en) * 2003-01-13 2003-07-23 浙江大学 Method for extracting tea polysaccharide from tailings with tea polyphenols being extracted
CN102060937A (en) * 2011-02-25 2011-05-18 余芳 Extraction and separation method for green tea polysaccharides
CN103819311A (en) * 2014-02-26 2014-05-28 成都华高生物制品有限公司 Method for extracting high-content tea polyphenol from fresh tea
CN104211824A (en) * 2014-08-27 2014-12-17 陕西盛迈石油有限公司 Preparation method of tea polysaccharide
CN105273103A (en) * 2015-11-12 2016-01-27 云南茶农生物产业有限责任公司 Method for preparing tea polysaccharides by combining separating membranes with chromatographic column
CN108440481A (en) * 2018-04-20 2018-08-24 佛山推启农业研究院(普通合伙) A kind of microwave combined method for extracting effective ingredient in thick tea of ultrasound-

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曹博: ""茶多酚、茶多糖和茶氨酸的综合提纯研究"", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 *
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Application publication date: 20190212