CN101519458A - Method for extracting tea polysaccharides and tea polyphenol from coarse old green tea - Google Patents
Method for extracting tea polysaccharides and tea polyphenol from coarse old green tea Download PDFInfo
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Abstract
A method for extracting tea polysaccharides and tea polyphenol from coarse old green tea comprises the following steps: extrusion treatment, extraction by deionized water, concentration, precipitation by ethanol, separation, vacuum freeze drying, and the like. The main difference between the method for extracting tea polysaccharides and tea polyphenol from coarse old green tea and the prior extracting method is that in the former one a single-screw extrusion machine is adopted to extrude material with optimum moisture content at optimum temperature so that the material is pretreated, then an aqueous extract method is utilized to obtain a general extract containing tea polysaccharides and tea polyphenol, and the tea polysaccharides is separated from the tea polyphenol in an alcohol deposition method. The extrusion treatment causes the organization structure of tea to be changed, thereby the yield coefficient of the tea polysaccharides and the tea polyphenol are high. Furthermore, under the extrusion action, the molecular structure of active ingredients in the tea is changed, thereby the activity can be reinforced. In addition, the coarse old green tea having plenteous source is utilized, thereby the serious waste of natural resources can be avoided. The method also has the advantage of simple technology.
Description
Technical field
The present invention relates to the extracting method of a kind of tea polysaccharide and tea-polyphenol, particularly relate to a kind of method of from thick old green tea, extracting tea polysaccharide and tea-polyphenol.
Background technology
The pharmaceutical use of tealeaves is with a long history, and according to putting down in writing in the Shennong's Herbal: obeying tealeaves for a long time can " makes one feel at ease and energetic, make light of one's life by commiting suicide anti-old ".Described in Tang's supplement to the Herbal: " all medicines are the medicine of each disease, and tea is the medicine of ten thousand diseases ".A large amount of studies show that contain the multiple bioactive ingredients that is utilized in the tealeaves, the main component that wherein has utility value has tea-polyphenol, tea polysaccharide and caffeine etc.
China produces about 100,000 tons of coarse tea per year, and along with the raising of living standards of the people, coarse tea more and more be nobody shows any interest in, so caused a large amount of overstocked stocks, therefore finally can only will cause a large amount of wastes of natural resources like this used as fertilizer or fuel.Yet compositions such as the tea polysaccharide that is rich in the coarse tea, tea-polyphenol have a wide range of applications aspect anti-oxidant, hypoglycemic.
Tea polysaccharide is an active substance important in the coarse tea, pharmacological research shows, multiple efficacies such as that tea polysaccharide has is hypoglycemic, reducing blood-fat, anticoagulation, antithrombotic, hypotensive, hypoxia tolerance, coronary blood flow increasing, radioprotective, enhancing body immunizing power, anticancer, anti-inflammatory, especially significant blood sugar decreasing effect and immunocompetence make it be expected to become the natural drug of prevent diabetes and cardiovascular disorder, strengthening immunity.
Tea-polyphenol is the natural product that extracts from tealeaves, has different physiological roles and nontoxic to human body, therefore is subjected in recent years paying close attention to widely.Because tea-polyphenol is a kind of natural anti-oxidation preservation agent of high-efficiency low-toxicity, thereby in foodstuffs industry, be mainly used in the fresh-keeping of grease and goods thereof, fried and bake, fish and meat product, and can replace synthetic antioxidant BHA, BHT commonly used in the present foodstuffs industry.In addition, that tea-polyphenol has aspect medical is antiviral, antibiotic, antibacterial, prevention of dental caries, improve renal function, reducing blood-fat, effect such as hypotensive, hypoglycemic, anti-oxidant, anticancer, and clinical study finds that tea-polyphenol has good action to alleviating the cardiovascular systems pathology.
Adopt at present usually extraction that water extraction ethanol sedimentation or solvent-extracted method carry out tea polysaccharide and tea-polyphenol in the coarse tea and separate, because conventional water extraction ethanol sedimentation extracting method yield is lower, the tea polysaccharide yield has only 2%～5%, the tea-polyphenol yield has only 15%～20%, and solvent extration can cause environmental pollution because of having used a large amount of organic solvents.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide a kind of yield height, and the extraction tea polysaccharide from thick old green tea that can enhanced activity and the method for tea-polyphenol.
In order to achieve the above object, provided by the invention from thick old green tea the method for extraction tea polysaccharide and tea-polyphenol comprise the following step that carries out in order:
1) in thick old green tea, is incorporated as the water of its quality 4%～12%, under 100 ℃～160 ℃ temperature, utilizes single-screw extrusion machine to push then, so that raw material is carried out pre-treatment;
2) above-mentioned thick old green tea through extrusion process is joined in the deionized water, the mass ratio of described thick old green tea and deionized water is 1: 5～1: 15, under 70 ℃～90 ℃ temperature, stir then and extracted 0.5～1.5 hour, lixiviate is 2～5 times repeatedly, filtration under diminished pressure afterwards merges filtrate and obtains containing the tealeaves test liquid of tea polysaccharide and tea-polyphenol;
3) under 40 ℃～60 ℃ temperature and the pressure of 0.06～0.1MPa, place Rotary Evaporators to be evaporated to 1/10～1/4 of original volume above-mentioned tealeaves test liquid, the dehydrated alcohol that adds 3～5 times of volumes then in the tealeaves test liquid after concentrating precipitates, left standstill 8～15 hours, centrifugation 6～10 minutes under 2000～4000 rev/mins rotating speed afterwards, collecting precipitation thing and supernatant liquor respectively; With the dehydrated alcohol of 2～3 times of volumes above-mentioned throw out is washed decolouring 3～5 times then, secondary precipitate is collected in centrifugation 6～10 minutes under 3000～4000 rev/mins rotating speed afterwards;
4) deionized water with 5～7 times of volumes dissolves the secondary precipitate of collecting in the step 3), places then to carry out freezingly under-18 ℃ the temperature, freezes the vacuum freeze drier that places-50 ℃ after real and carries out drying and can obtain the tea polysaccharide product;
5) supernatant liquor that obtains in step 3) under 30 ℃～40 ℃ temperature and the pressure of 0.06～0.1MPa places Rotary Evaporators to be evaporated to 1/10～1/4 of original volume, place then and carry out freezingly under-18 ℃ the temperature, freeze the vacuum freeze drier that places-50 ℃ after real and carry out drying and can obtain the tea-polyphenol product.
Amount of water in the described step 1) is 4%～8%.
Temperature range in the described step 1) is 100 ℃～130 ℃.
The method of extracting tea polysaccharide and tea-polyphenol from thick old green tea provided by the invention is distinguished with the maximum of existing extracting method and is that the present invention adopts single-screw extrusion machine under moisture that suits and temperature condition raw material to be pushed earlier, so that raw material is carried out pre-treatment, utilize water extraction to obtain to contain the general extractive of tea polysaccharide and tea-polyphenol then, separate tea polysaccharide and tea-polyphenol with alcohol deposition method again.Because extrusion process makes the tealeaves weave construction change, thereby the yield height of tea polysaccharide and tea-polyphenol, and under the effect of extruding, the structure of activeconstituents molecule can change in the tealeaves, therefore can make its increased activity.In addition, because it is sufficient to originate as the thick old green tea of raw material, it is used also can avoids a large amount of wastes of natural resources.In addition, present method also has advantage of simple technology.
Description of drawings
Fig. 1 is tea polysaccharide and the tea-polyphenol yield histogram that utilizes method provided by the invention and existing extracting method to extract from thick old green tea.Wherein TPS represents tea polysaccharide, and TP represents tea-polyphenol, the water weight that the per-cent in the X-coordinate adds during for extrusion process, the temperature value when temperature is extrusion process.Control group is tea polysaccharide and the tea-polyphenol that is obtained when extracting method extracts according to having now.
Embodiment
Below in conjunction with specific embodiment the method for extracting tea polysaccharide and tea-polyphenol from thick old green tea provided by the invention is elaborated.
Embodiment 1:
1) in thick old green tea, is incorporated as the water of its quality 4%, under 130 ℃ temperature, utilizes single-screw extrusion machine to push then, so that raw material is carried out pre-treatment;
2) above-mentioned thick old green tea through extrusion process is joined in the deionized water, the mass ratio of described thick old green tea and deionized water is 1: 10, under 80 ℃ temperature, stir then and extracted 0.5 hour, lixiviate is 3 times repeatedly, filtration under diminished pressure afterwards merges filtrate and obtains containing the tealeaves test liquid of tea polysaccharide and tea-polyphenol;
3) under the pressure of 50 ℃ temperature and 0.09MPa, place Rotary Evaporators to be evaporated to 1/4 of original volume above-mentioned tealeaves test liquid, the dehydrated alcohol that adds 3 times of volumes then in the tealeaves test liquid after concentrating precipitates, left standstill 12 hours, centrifugation 8 minutes under 2500 rev/mins rotating speed afterwards, collecting precipitation thing and supernatant liquor respectively; With the dehydrated alcohol of 3 times of volumes above-mentioned throw out is washed decolouring 5 times then, secondary precipitate is collected in centrifugation 7 minutes under 3000 rev/mins rotating speed afterwards;
4) deionized water with 7 times of volumes dissolves the secondary precipitate of collecting in the step 3), place then carry out under-18 ℃ the temperature freezing, freezing the vacuum freeze drier that places-50 ℃ after real carries out drying and can obtain the tea polysaccharide product, yield is 6.6%, and the content of measuring tea polysaccharide in this product through phenol-sulfuric acid process is 30.4%;
5) supernatant liquor that obtains in step 3) under the pressure of 35 ℃ temperature and 0.09MPa places Rotary Evaporators to be evaporated to 1/4 of original volume, place then carry out under-18 ℃ the temperature freezing, freezing the vacuum freeze drier that places-50 ℃ after real carries out drying and can obtain the tea-polyphenol product, yield is 26.5%, and the content of tea-polyphenol is 65.3% in this product of ferrous tartrate colorimetric method for determining.
Embodiment 2:
1) in thick old green tea, is incorporated as the water of its quality 8%, under 100 ℃ temperature, utilizes single-screw extrusion machine to push then, so that raw material is carried out pre-treatment;
2) above-mentioned thick old green tea through extrusion process is joined in the deionized water, the mass ratio of described thick old green tea and deionized water is 1: 5, under 70 ℃ temperature, stir then and extracted 1.5 hours, lixiviate is 4 times repeatedly, filtration under diminished pressure afterwards merges filtrate and obtains containing the tealeaves test liquid of tea polysaccharide and tea-polyphenol;
3) under the pressure of 45 ℃ temperature and 0.09MPa, place Rotary Evaporators to be evaporated to 1/8 of original volume above-mentioned tealeaves test liquid, the dehydrated alcohol that adds 3 times of volumes then in the tealeaves test liquid after concentrating precipitates, left standstill 8 hours, centrifugation 6 minutes under 3500 rev/mins rotating speed afterwards, collecting precipitation thing and supernatant liquor respectively; With the dehydrated alcohol of 3 times of volumes above-mentioned throw out is washed decolouring 3 times then, secondary precipitate is collected in centrifugation 6 minutes under 3500 rev/mins rotating speed afterwards;
4) deionized water with 6 times of volumes dissolves the secondary precipitate of collecting in the step 3), place then carry out under-18 ℃ the temperature freezing, freezing the vacuum freeze drier that places-50 ℃ after real carries out drying and can obtain the tea polysaccharide product, yield is 8.7%, and the content of measuring tea polysaccharide in this product through phenol-sulfuric acid process is 17.9%;
5) supernatant liquor that obtains in step 3) under the pressure of 30 ℃ temperature and 0.1MPa places Rotary Evaporators to be evaporated to 1/6 of original volume, place then carry out under-18 ℃ the temperature freezing, freezing the vacuum freeze drier that places-50 ℃ after real carries out drying and can obtain the tea-polyphenol product, yield is 24.5%, and the content of tea-polyphenol is 64.4% in this product of ferrous tartrate colorimetric method for determining.
The inventor will utilize the tea polysaccharide that method that the invention described above provides and existing extracting method extract and the yield drafting pattern of tea-polyphenol from thick old green tea, the results are shown in Figure 1.
In addition, the inventor tests the tea polysaccharide that method obtained of extracting tea polysaccharide and tea-polyphenol from thick old green tea, the tea-polyphenol removing DPPH. free radical ability of utilizing the foregoing description to provide.
Free radical is to have highly chemically active material, it is the intermediate product of multiple biochemical reaction in the vital movement, people's vital movement be unable to do without free radical, but the interior free radical of human body is too much or removed slow, macromole can be attacked and damage to free radical then, cell membrane, nucleic acid and body protein etc. cause damage, be cause human senility, cause a disease, one of carcinogenic important factor.
Removing the DPPH free radical tests employed tea polysaccharide and all adopts with tea-polyphenol and have 2 kinds of different extrusion process conditions the present method of (the adding water yield and extrusion temperature) obtains, and contrast with the tea polysaccharide that existing method obtained and the tea-polyphenol that do not carry out extrusion process, experimental result sees Table 1:
Tea polysaccharide and tea-polyphenol contrast and experiment that table 1 utilizes present method and existing method to obtain
By above-mentioned experimental result as can be seen, compare with tea-polyphenol, utilize tea polysaccharide that the inventive method obtains and tea-polyphenol that the removing ability of DPPH free radical all is enhanced with the tea polysaccharide that existing method obtained of not carrying out extrusion process.
Claims (3)
1, a kind of method of extracting tea polysaccharide and tea-polyphenol from thick old green tea is characterized in that: the described method of extracting tea polysaccharide and tea-polyphenol from thick old green tea comprises the following step that carries out in order:
1) in thick old green tea, is incorporated as the water of its quality 4%～12%, under 100 ℃～160 ℃ temperature, utilizes single-screw extrusion machine to push then, so that raw material is carried out pre-treatment;
2) above-mentioned thick old green tea through extrusion process is joined in the deionized water, the mass ratio of described thick old green tea and deionized water is 1: 5～1: 15, under 70 ℃～90 ℃ temperature, stir then and extracted 0.5～1.5 hour, lixiviate is 2～5 times repeatedly, filtration under diminished pressure afterwards merges filtrate and obtains containing the tealeaves test liquid of tea polysaccharide and tea-polyphenol;
3) under 40 ℃～60 ℃ temperature and the pressure of 0.06～0.1MPa, place Rotary Evaporators to be evaporated to 1/10～1/4 of original volume above-mentioned tealeaves test liquid, the dehydrated alcohol that adds 3～5 times of volumes then in the tealeaves test liquid after concentrating precipitates, left standstill 8～15 hours, centrifugation 6～10 minutes under 2000～4000 rev/mins rotating speed afterwards, collecting precipitation thing and supernatant liquor respectively; With the dehydrated alcohol of 2～3 times of volumes above-mentioned throw out is washed decolouring 3～5 times then, secondary precipitate is collected in centrifugation 6～10 minutes under 3000～4000 rev/mins rotating speed afterwards;
4) deionized water with 5～7 times of volumes dissolves the secondary precipitate of collecting in the step 3), places then to carry out freezingly under-18 ℃ the temperature, freezes the vacuum freeze drier that places-50 ℃ after real and carries out drying and can obtain the tea polysaccharide product;
5) supernatant liquor that obtains in step 3) under 30 ℃～40 ℃ temperature and the pressure of 0.06～0.1MPa places Rotary Evaporators to be evaporated to 1/10～1/4 of original volume, place then and carry out freezingly under-18 ℃ the temperature, freeze the vacuum freeze drier that places-50 ℃ after real and carry out drying and can obtain the tea-polyphenol product.
2, the method for extracting tea polysaccharide and tea-polyphenol from thick old green tea according to claim 1, it is characterized in that: the amount of water in the described step 1) is 4%～8%.
3, the method for extracting tea polysaccharide and tea-polyphenol from thick old green tea according to claim 1, it is characterized in that: the temperature range in the described step 1) is 100 ℃～130 ℃.
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| CN101843310A (en) * | 2010-04-30 | 2010-09-29 | 浙江省医学科学院 | Jiantangcha (blood glucose benefiting tea) capsule for adjunctively reducing blood glucose and improving symptoms of diabetes and preparation method thereof |
| CN101921345A (en) * | 2010-08-13 | 2010-12-22 | 南昌大学 | Method for extracting polysaccharide and flavone from bamboo leaves |
| CN102336841A (en) * | 2011-10-18 | 2012-02-01 | 中国计量学院 | Method for extracting tea polysaccharide |
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| CN103450365A (en) * | 2012-07-05 | 2013-12-18 | 陈小强 | Method for purifying and preparing tea polysaccharide composite through high-speed countercurrent chromatography technology |
| CN103833863A (en) * | 2012-11-20 | 2014-06-04 | 中国科学院兰州化学物理研究所 | Technology for preparing crude polysaccharides by extracting polysaccharides from Enteromorpha prolifera |
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| CN110663789A (en) * | 2019-11-17 | 2020-01-10 | 横县振茂茶厂 | Method for extracting tea polyphenol by taking tea hair as raw material |
| CN116270851A (en) * | 2023-04-10 | 2023-06-23 | 中国检验检疫科学研究院 | Preparation method of Dahongpao extract and application of Dahongpao extract in antihypertensive drugs or foods |
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| CN101843310A (en) * | 2010-04-30 | 2010-09-29 | 浙江省医学科学院 | Jiantangcha (blood glucose benefiting tea) capsule for adjunctively reducing blood glucose and improving symptoms of diabetes and preparation method thereof |
| CN101843310B (en) * | 2010-04-30 | 2013-03-13 | 浙江省医学科学院 | Jiantangcha (blood glucose benefiting tea) capsule for assistantly reducing blood glucose and improving symptoms of diabetes and preparation method thereof |
| CN101921345A (en) * | 2010-08-13 | 2010-12-22 | 南昌大学 | Method for extracting polysaccharide and flavone from bamboo leaves |
| CN102336841B (en) * | 2011-10-18 | 2013-09-18 | 中国计量学院 | Method for extracting tea polysaccharide |
| CN102336841A (en) * | 2011-10-18 | 2012-02-01 | 中国计量学院 | Method for extracting tea polysaccharide |
| CN103450365A (en) * | 2012-07-05 | 2013-12-18 | 陈小强 | Method for purifying and preparing tea polysaccharide composite through high-speed countercurrent chromatography technology |
| CN102919424B (en) * | 2012-11-15 | 2014-02-26 | 戴群 | Pu'er raw tea extract for effectively retaining quality of original tea and preparation method |
| CN102919424A (en) * | 2012-11-15 | 2013-02-13 | 戴群 | Pu'er raw tea extract for effectively retaining quality of original tea and preparation method and application of same |
| CN102919426A (en) * | 2012-11-15 | 2013-02-13 | 戴群 | Pu'er tea extract for effectively retaining original tea aroma and taste and preparation method and application of same |
| CN102919426B (en) * | 2012-11-15 | 2014-10-29 | 戴群 | Pu'er tea extract for effectively retaining original tea aroma and taste and preparation method |
| CN103833863A (en) * | 2012-11-20 | 2014-06-04 | 中国科学院兰州化学物理研究所 | Technology for preparing crude polysaccharides by extracting polysaccharides from Enteromorpha prolifera |
| CN106332990A (en) * | 2016-08-24 | 2017-01-18 | 王志远 | Activated tea powder using coarse old tea leaf as raw material, and preparation method thereof |
| CN107573429A (en) * | 2016-11-21 | 2018-01-12 | 广西大学 | A kind of method that jasmine tea tea polysaccharide is extracted using the precipitation method |
| CN107279369A (en) * | 2017-06-07 | 2017-10-24 | 安徽农业大学 | A kind of preparation method of hypoglycemic yellow tea |
| CN107937199A (en) * | 2018-01-21 | 2018-04-20 | 胡江宇 | A kind of green tea preparation of wine |
| CN108250316A (en) * | 2018-02-06 | 2018-07-06 | 信阳师范学院 | A kind of extracting method of tea polysaccharide |
| CN110663789A (en) * | 2019-11-17 | 2020-01-10 | 横县振茂茶厂 | Method for extracting tea polyphenol by taking tea hair as raw material |
| CN116270851A (en) * | 2023-04-10 | 2023-06-23 | 中国检验检疫科学研究院 | Preparation method of Dahongpao extract and application of Dahongpao extract in antihypertensive drugs or foods |
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