CN106065036B - A kind of method of hydro-thermal method extraction tea polysaccharide - Google Patents
A kind of method of hydro-thermal method extraction tea polysaccharide Download PDFInfo
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- CN106065036B CN106065036B CN201610569828.8A CN201610569828A CN106065036B CN 106065036 B CN106065036 B CN 106065036B CN 201610569828 A CN201610569828 A CN 201610569828A CN 106065036 B CN106065036 B CN 106065036B
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- tea
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- tea polysaccharide
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 31
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 31
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000000605 extraction Methods 0.000 title claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 7
- 241001122767 Theaceae Species 0.000 title 1
- 244000269722 Thea sinensis Species 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 235000009024 Ceanothus sanguineus Nutrition 0.000 claims abstract description 3
- 240000003553 Leptospermum scoparium Species 0.000 claims abstract description 3
- 235000015459 Lycium barbarum Nutrition 0.000 claims abstract description 3
- 238000000502 dialysis Methods 0.000 claims description 16
- 238000001694 spray drying Methods 0.000 claims description 10
- 239000012141 concentrate Substances 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000002386 leaching Methods 0.000 abstract description 7
- 238000001035 drying Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 235000013616 tea Nutrition 0.000 description 36
- 239000000243 solution Substances 0.000 description 13
- 102000004190 Enzymes Human genes 0.000 description 4
- 108090000790 Enzymes Proteins 0.000 description 4
- 238000003809 water extraction Methods 0.000 description 3
- 230000002255 enzymatic effect Effects 0.000 description 2
- 208000001953 Hypotension Diseases 0.000 description 1
- 230000002785 anti-thrombosis Effects 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 230000010100 anticoagulation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 208000021822 hypotensive Diseases 0.000 description 1
- 230000001077 hypotensive effect Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010563 solid-state fermentation Methods 0.000 description 1
- 235000020334 white tea Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General 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 invention discloses a kind of method of hydro-thermal method extraction tea polysaccharide, its step includes：(1) after drying raw material tea leaf, tea tree branch, tea processing residue or tea processing discarded object, 40~60 mesh are crushed to；(2) the volume L with water, it is 0.5~2.0h of stirring and leaching under 1: 10~1: 30,120~200 DEG C of temperature, 0.1~2.5MPa of pressure according to mass volume ratio using high-temperature high-pressure reaction kettle by the material quality kg after crushing；(3) leaching liquor separation, concentration, dry obtained tea polysaccharide.Compared with prior art, operating process of the present invention is easy, safe, and without using organic solvent, and yield is higher.
Description
Technical field
The present invention relates to a kind of Tea Polysaccharides extracting method, a kind of method that tea polysaccharide is extracted more particularly to hydro-thermal method,
Belong to field of chemical engineering.
Background technology
Tea polysaccharide has good physicochemical property and significant physiologically active is for example hypoglycemic, reducing blood lipid, hypotensive, enhancing are exempted from
The effect such as epidemic disease power, anticoagulation, antithrombotic and resist oxygen lack and treatment diabetes, tea polysaccharide is as natural drug, life in recent years
Thing chemistry, the study hotspot of life science.Because it is widely applied basis, therefore the extraction separation of tea polysaccharide becomes outstanding
For key.
At present, the extracting method of tea polysaccharide mainly has Hot water extraction (≤100 DEG C) or enzyme formulation etc., such as prior art
A kind of method of the separation and Extraction natural tea polysaccharide at a temperature of 5-75 DEG C disclosed in CN201010141786.0,
One kind disclosed in CN201110332109.1 extracts tea polysaccharide method at a temperature of 85 DEG C, and the tea that above Hot water extraction obtains is more
Sugared yield is relatively low.One kind disclosed in CN201410138882.8 accesses the extraction of strain substep solid state fermentation in tea leaf powder or tea seed cake
Traditional water extraction and modern enzyme engineering are combined extraction Polysaccharide from Green Tea by the method for tea polysaccharide, one kind disclosed in CN201510876422.X
Method, above enzyme extraction method because enzyme has selectivity and selectivity, extraction when should be noted pH value, hydrolysis temperature and enzymolysis
The factors such as time, so as to limit large-scale use Enzymatic Extraction tea polysaccharide.
Therefore, adopted for above-mentioned hot-water process and the deficiency of Enzymatic Extraction tea polysaccharide, this patent in high-temperature high-pressure reaction kettle
Tea polysaccharide is extracted with hydro-thermal method (100 DEG C of ＞), i.e., makes the quick complete molten extraction tealeaves of Tea Polysaccharides using the aqueous solution of HTHP
Polysaccharide, Tea Polysaccharides yield can be effectively improved.
The content of the invention
It is an object of the invention to provide a kind of new and effective tea polysaccharide extracting method.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method of hydro-thermal method extraction tea polysaccharide, comprises the following steps：
(1) by after raw material stoving, 40~60 mesh are crushed to；
(2) it is 1: 10~1: 30 by the sample after step (1) described crushing and the mass volume ratio of water, in high temperature high pressure reverse
Answer 0.1~2.5MPa of pressure in kettle, 0.5~2.0h of stirring reaction at 120~200 DEG C of temperature, the unit of the quality is kg, institute
The unit for stating volume is L；
(3) step (2) extract solution is filtered or centrifuged；
(4) step (3) filtered fluid or centrifugate are dialysed using bag filter；
(5) solution after step (4) described dialysis is concentrated by evaporation to 30~40%；
(6) step (5) concentrate is spray-dried, obtains tea polysaccharide.
Further to realize the object of the invention, raw material described in step (1) is tealeaves, tea tree branch, tea processing residue or
It is any in tea processing discarded object.
Step (3) described centrifugal rotational speed is 1000~5000rpm/min, and centrifugation time is 5~20min.
From the bag filter that molecular cut off is 3~150kDa, dialysis time is 1~3 day for step (4) dialysis.
Described be concentrated by evaporation of step (5) concentrates for system of three-effect downstream evaporator, and an effect pressure is 0.05~1.0MPa, temperature 100
~110 DEG C, concentration is 5~8%, and two effect pressure are 0MPa, and 100~110 DEG C of temperature, concentration is 20~25%, triple effect pressure-
0.004~-0.005MPa, temperature are 100~110 DEG C, and concentration is 30~40%.
Spray drying described in step (6) is pressure spray dryer, appointing in centrifugal spray drying, pneumatic spray drying
Meaning is a kind of.
Beneficial effect
Compared with prior art, operating process of the present invention is easy, safe, and without using organic solvent, tea polysaccharide yield can carry
It is high by 10~20%.
Embodiment
The present invention is further illustrated with reference to case study on implementation, but the implementation of the present invention is not limited to this.
Embodiment 1
(1) by after DAYEWULONG drying tea leaves, 40~60 mesh are crushed to；
(2) sample after step (1) described crushing is weighed into 1kg, be added in 10L water, in 120 DEG C of temperature, pressure
Stirring and leaching 2.0h under 0.1MPa；
(3) step (2) extract solution is filtered；
(4) step (3) described filtered fluid is subjected to dialysis 1 day using 3kDa bag filter；
(5) solution after step (4) described dialysis is concentrated into 30% using system of three-effect downstream evaporator；
(6) step (5) the concentrate centrifugal spray drying is produced into tea polysaccharide, yield 5.5%.
Embodiment 2
(1) by after No. 1 drying tea leaves of Shan tea, 40~60 mesh are crushed to；
(2) sample after step (1) described crushing is weighed into 1kg, be added in 30L water, in 200 DEG C of temperature, pressure
2.5MPa stirring and leachings 0.5h；
(3) step (2) described extract solution is centrifuged into 20min under rotating speed 1000rpm/min；
(4) step (3) described centrifugate is subjected to dialysis 2 days using 4kDa bag filter；
(5) solution after step (4) described dialysis is concentrated into 35% using system of three-effect downstream evaporator：
(6) step (5) the concentrate pressure spray dryer is produced into tea polysaccharide, yield 7.2%.
Embodiment 3
(1) by after the drying tea leaves of Dragon Well tea 43,40~60 mesh are crushed to；
(2) sample after step (1) described crushing is weighed into 1kg, be added in 20L water, in 140 DEG C of temperature, pressure
Stirring and leaching 1.5h under 0.5Mpa；
(3) step (2) described extract solution is centrifuged into 5min under rotating speed 5000rpm/min；
(4) step (3) described centrifugate is subjected to dialysis 3 days using 150kDa bag filter；
(5) solution after step (4) described dialysis is concentrated into 40% using system of three-effect downstream evaporator；
(6) step (5) the concentrate pneumatic spray drying is produced into tea polysaccharide, yield 4.1%.
Embodiment 4
(1) after Fuding white tea leaf is dried, 40~60 mesh are crushed to；
(2) sample after step (1) described crushing is weighed into 1kg, be added in 25L water, in 160 DEG C of temperature, pressure
Stirring and leaching 1.0h under 1.0MPa；
(3) step (2) extract solution is filtered；
(4) step (3) described filtered fluid is subjected to dialysis 2 days using 70kDa bag filter；
(5) solution after step (4) described dialysis is concentrated into 32% using system of three-effect downstream evaporator；
(6) step (5) the concentrate centrifugal spray drying is produced into tea polysaccharide, yield 6.8%.
Embodiment 5
(1) by after the middle drying tea leaves of tea 108,40~60 mesh are crushed to；
(2) sample after step (1) described crushing is weighed into 1kg, be added in 15L water, in 180 DEG C of temperature, pressure
Stirring and leaching 1.2h under 2.0MPa；
(3) step (2) extract solution is filtered；
(4) step (3) described filtered fluid is subjected to dialysis 1 day using 10kDa bag filter；
(5) solution after step (4) described dialysis is concentrated into 38% using system of three-effect downstream evaporator；
(6) step (5) the concentrate centrifugal spray drying is produced into tea polysaccharide, yield 7.5%.
Claims (1)
- A kind of 1. method of hydro-thermal method extraction tea polysaccharide, it is characterised in that comprise the following steps that：(1) by after raw material stoving, 60 mesh are crushed to；(2) it is 1 by the sample after step (1) described crushing and the mass volume ratio of water:10~1:20, in high-temperature high-pressure reaction kettle Middle 0.5~2.5MPa of pressure, stirring reaction 2.0h at 160~200 DEG C of temperature, the unit of the quality is kg, the volume Unit is L；(3) step (2) extract solution is filtered or centrifuged；(4) step (3) filtered fluid or centrifugate are dialysed using bag filter；(5) solution after step (4) described dialysis is concentrated by evaporation to 30~40%；(6) step (5) concentrate is spray-dried, obtains tea polysaccharide；Raw material described in step (1) is any in tealeaves, tea tree branch, tea processing residue or tea processing discarded object；Step (3) described centrifugal rotational speed is 1000~5000rpm, and centrifugation time is 5~20min；From the bag filter that molecular cut off is 3~150kDa, dialysis time is 1~3 day for step (4) dialysis；Described be concentrated by evaporation of step (5) concentrates for system of three-effect downstream evaporator, and an effect pressure is 0.05~1.0MPa, temperature 100~110 DEG C, concentration is 5~8%, and two effect pressure are 0MPa, and 100~110 DEG C of temperature, concentration is 20~25%, triple effect pressure -0.004 ~-0.005MPa, temperature are 100~110 DEG C, and concentration is 30~40%；Spray drying described in step (6) is any one in pressure spray dryer, centrifugal spray drying, pneumatic spray drying Kind.
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| CN106478835A (en) * | 2016-11-22 | 2017-03-08 | 广西钱隆投资管理有限公司 | A kind of extracting method of tea polysaccharide |
| CN109142591A (en) * | 2018-11-06 | 2019-01-04 | 国家烟草质量监督检验中心 | The hydro-thermal extracting method and Liquid Chromatography-Tandem Mass Spectrometry measuring method of maleic hydrazide are remained in a kind of tobacco |
| CN114904293A (en) * | 2022-05-05 | 2022-08-16 | 泉州市金斗洋生态农业股份有限责任公司 | Batch recycling and extracting process for oolong tea leaves |
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| CN103059150A (en) * | 2011-10-22 | 2013-04-24 | 徐玮 | Process for extracting tea polysaccharide by water process |
| CN102746415B (en) * | 2012-07-28 | 2014-03-26 | 江南大学 | Method for simultaneously extracting tea polysaccharide and tea polyphenol with subcritical water |
| CN105582170A (en) * | 2014-10-23 | 2016-05-18 | 陆道华 | A comprehensive utilization method for low-grade tea leaves |
| CN104592410B (en) * | 2015-01-14 | 2017-02-01 | 宁夏森淼种业生物工程有限公司 | Method for efficiently extracting polysaccharide of lycium barbarum leaves |
| CN104725522A (en) * | 2015-03-31 | 2015-06-24 | 高枫 | Method for extracting white fungus polysaccharides at high temperature under high pressure |
| CN105061622B (en) * | 2015-08-07 | 2019-07-09 | 贵州科睿捷信息技术有限公司 | A kind of extraction process of tea polysaccharide |
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Effective date of registration: 20240605 Address after: No. 18 Chayi Street, Shangnan County, Shangluo City, Shaanxi Province, 726399 Patentee after: Shaanxi Shangnan tea joint venture Co. Country or region after: China Address before: 712100 Xianyang city of Shaanxi province Yangling Demonstration Zone No. 3 Tai Road Patentee before: NORTHWEST A & F University Country or region before: China |