CN103992359A - Preparation process for extracting green tea polyphenols from tea - Google Patents
Preparation process for extracting green tea polyphenols from tea Download PDFInfo
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Abstract
Belonging to the field of green tea polyphenol extraction processes, the invention discloses a preparation process for extracting green tea polyphenols from tea. The preparation process includes the following six steps: pretreatment of tea, nitrogen protection, ultrasonic extraction, separation and filtration, resin adsorption, concentration and drying. The process provided by the invention solves the problems of serious destruction of effective components, low product yield and purity, high production cost and pollution in existing green tea polyphenol extraction. The preparation method disclosed in the invention not only has the advantages of high recovery rate, time saving, high extraction rate and the like, but also avoids the use of toxic solvents, and is conducive to reducing energy consumption and lowering the production cost, thus having good industrial promotion value.
Description
Technical field
The present invention relates to process for extracting tea polyphenol field, particularly a kind of preparation technology who extracts tea-polyphenol from tealeaves.
Background technology
Tourism industry tea is gained the name because producing tourism industry.Tourism industry is close to Xun Jiang, and famous newborn current of spring is by tea place, and spring profit mist holds together, the growth of very suitable tea tree.It originates from the Tang Dynasty, to the well-known Guangdong and Guangxi Provinces of the Ming Dynasty and Hunan, Fujian and other places.According to < <, record as mansion, state will > >: " Western Hills tea, look clear is green and taste is fragrant, does not subtract Dragon Well tea." pass on from one to another, Western Hills temple Buddhist monks and nums introduce tea tree seed by the south of the River, make to produce Western Hills tea here.The highly skilled person of Western Hills tea frying is still the Western Hills Buddhist nunnery Buddhist nun of institute.Afterwards by poor management, Western Hills tea is on the brink of extinction, and wide energy Master in 1949 is released the huge Master of praising and recommends, come Guiping County Western Hills and preside over Buddhism affairs, simultaneously with releasing together with prosperous intelligent Master of newly becoming a Buddhist monk or nun, at chessboard stone, wash the ground such as stone Buddhist nunnery kind of the tea of opening up wasteland, Western Hills tea is obtained newborn.
Tea-polyphenol (Green Tea Polyphenols is called for short GTP) is the general name of Catechin in Tea class, flavonoid, phenolic acids and anthocyan compound, accounts for the 15%-25% of dry weight of tea leaves.In tea-polyphenol, most important composition is the multiple catechin (catechins) of flavanol compound.In tea-polyphenol molecule, with a plurality of activity hydroxies (OH), can stop free chain reaction in human body, remove superoxide ion, the effect of similar SOD, tea-polyphenol reaches more than 98% the elimination factor of superoxide anion and hydrogen peroxide free radical, be significant dose-effect relationship, its effect is better than vitamin-E and C; Tea-polyphenol cell membrane and cell walls have provide protection, fairly obvious to the elimination effect of lipid peroxidation free radical.Tea-polyphenol is antibacterial, tea bacterium effect in addition, can effectively reduce the absorption of large intestine to cholesterol, prevents and treats atherosclerosis, it is the strong inhibition of virus of AIDS (HIV) Revertase, have enhancing body immunological competence, antitumor, radioprotective, has resisting oxidation and delaying senility mechanism.Toxicologic study confirmation, tea-polyphenol is safe, nontoxic.Tea-polyphenol has broad application prospects in all many-sides such as medicine, daily use chemicals, lightization, makeup, food, grease, health cares.
The researchdevelopment of tea-polyphenol, the eighties, enters the nineties and forms climax.At present the purification of tea-polyphenol and applied research are received to concern both domestic and external, still in the stage in the ascendant.The medicine of tea-polyphenol and health care are worth, tea-polyphenol has become the focus of medicine, the exploitation of food circle, except tea-polyphenol tablet, capsule etc., as antioxidant and foodstuff additive, in the multiclass food such as oil and foodstuffs, ready-to-eat, fishery products, meat product, preparation, seasonings, candy, beverage, be all widely used at present.Therefore, there is the larger market requirement.
The method that has now several extraction tea-polyphenol:
Solvent-extraction process is to leach from tealeaves with polar solvent, then leaching liquid is carried out to liquid-liquid extraction separation, finally concentrates and obtain product.Suitability for industrialized production tea-polyphenol mainly adopts this method at present.Product yield is 5%-10%, and the purity of product is about 80%-98%, caffeine 4%-7%.Organic solvent used is as acetone, ether, methyl alcohol, ethane and trichloromethane etc.The method is used multiple organic solvent, and production cost is high, and the organic solvent of some toxic substance makes product safe not to the utmost with operation, and easily causes environmental pollution.
Ion precipitation method is to utilize metal can precipitate tea-polyphenol, and makes it separated with trimethyl-xanthine, as mantoquita, lead salt or aluminum chloride.The method has been used the poisonous heavy metal of human body has been made to precipitation agent, and its product can not be accepted for food food and medicine is industrial.
The equipment of the extensive consecutive production of resin adsorption method lacks, and is only suitable in production in a small amount; Sorbent material that need to be to the strong high adsorption capacity of tea-polyphenol selectivity, and sorbent material large usage quantity, and because protein, polysaccharide etc. in tealeaves easily stop up resin space, cause resin inactivation, resin activation and regenerate cumbersomely, resin price is high, invests larger.
Supercritical extraction, although the purity of extracting is high, extraction yield is extremely low, high to equipment requirements, investment is large, so large-scale industrial production also exists a lot of difficulties.
Summary of the invention
The object of the invention is to: for the problem of above-mentioned existence, provide a kind of preparation technology who extracts tea-polyphenol from tealeaves, solve while extracting tea-polyphenol at present that effective constituent is destroyed serious, product yield and purity is low, production cost is high and pollution problem.
The technical solution used in the present invention is as follows:
The preparation technology who extracts tea-polyphenol from tealeaves, comprises the following steps:
Step 1, tealeaves pre-treatment: choose high-quality tea, for tourism industry tealeaves, pulverize after oven dry, cross 60～80 mesh sieves, obtain tea powder;
Step 2, nitrogen protection: the tea powder of step 1 is placed in extraction kettle, adds distilled water fully to mix, feed liquid mass ratio is 1:6～1:15, uses vacuum pump deoxidation, then passes into pure nitrogen gas;
Step 3, supersound extraction: pass into after nitrogen, constant temperature carries out ultrasonic extraction, obtains the tea-polyphenol solution that contains residue;
Step 4, separation: by separator, the tea-polyphenol solution that contains residue in step 3 is filtered, separation obtains extracting solution and filter residue;
Step 5, resin absorption: with the tea-polyphenol of extracting solution in polyamide resin or NKA macroporous resin adsorption step 4, obtain resin and the waste liquid of Adsorption of Tea Polyphenols, then adopt 3 * 10
-4mol/L tartaric acid solution and 85% edible alcohol solution carry out wash-out to the resin of Adsorption of Tea Polyphenols, obtain tea-polyphenol elutriant;
Step 6, concentrate drying: tea-polyphenol elutriant is carried out to concentrated frozen and be dried, obtain tea-polyphenol finished product.
As preferred version of the present invention, described step 3 ultrasonic extraction condition is 20～50 ℃, extracts each 10～20min 1～3 time.
Preferably, the step 3 of returning to the filter residue that described step 4 separation obtains again repeats to extract.
Preferably, in described step 5, waste liquid adsorbs by resin again, returns to step 3 again and repeat to extract after removal impurity.
Preferably, while adding distilled water in described step 2, also can add again organic solvent.
Preferably, described in step 1, drying is that tealeaves is being placed in baker, dries to ridity and reach 98% at the temperature of 70～100 ℃.
In sum, the invention has the beneficial effects as follows:
1, ultrasonic extraction, carries out intensified by ultrasonic wave processing to leaching process, is to utilize hyperacoustic Mechanical Crushing and cavatition, accelerates tea-polyphenol extractive substance speed to solvent diffusion from tealeaves, shortens extraction time, increases the extraction yield of effective constituent.The condition of extracting, both guaranteed volatile, easily low-temperature short-time spoiled, material easy to change extracts, and has guaranteed again the time, obtains reservation and the high extraction high density tea juice of color, smell and taste.There is technique simple, extract that temperature is low, the rate of recovery is high, oxidation loss is little, during joint, energy-conservation, extraction yield advantages of higher, avoided the use of noxious solvent simultaneously, there is good industrial promotional value.
2, pass into pure nitrogen gas (concentration of nitrogen is more than 99%), supersound extraction is obtained to oxidizable tea-polyphenol and protect, in this condition leaching yield, significantly improve, and quality of finished is high.When the protection of nitrogen makes supersound extraction tea-polyphenol, not only reduced leaching temperature and shortened leaching time, and be conducive to reduce energy waste and reduce production costs.
3, waste liquid and waste residue recycle, improve the extraction yield of tealeaves, and sewage flow rate is less, not only economy but also can protection of the environment.Finally produce useless waste material waste residue and can also obtain other byproducts except tea-polyphenol, especially tea grounds can also be made organic composite fertilizer through biological treatment.
4, polymeric amide or NKA macroporous resin all have good adsorption effect, and adsorption rate can reach more than 85%, effectively removes the impurity such as vegetable polysaccharides, trimethyl-xanthine, has improved the DNA purity of tea-polyphenol, reaches 95%, has simplified extraction process.Adopt 80% ethanol as eluent, it is convenient to reclaim, environmentally safe.
5, utilize method of the present invention, extract tea-polyphenol, extraction yield can reach more than 26%, and purity reaches more than 95%, the trimethyl-xanthine < 2% in tea-polyphenol.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of the present invention.
Embodiment
The invention provides a kind of preparation technology who extracts tea-polyphenol from tea, comprise the following steps:
Step 1, tealeaves pre-treatment: choose high-quality tea, for tourism industry tealeaves, pulverize after oven dry, cross 60～80 mesh sieves, obtain tea powder;
Step 2, nitrogen protection: the tea powder of step 1 is placed in extraction kettle, adds distilled water fully to mix, feed liquid mass ratio is 1:6～1:15, uses vacuum pump deoxidation, then passes into pure nitrogen gas;
Step 3, supersound extraction: pass into after nitrogen, constant temperature carries out ultrasonic extraction, obtains the tea-polyphenol solution that contains residue;
Step 4, separation: by separator, the tea-polyphenol solution that contains residue in step 3 is filtered, separation obtains extracting solution and filter residue;
Step 5, resin absorption: with the tea-polyphenol of extracting solution in polyamide resin or NKA macroporous resin adsorption step 4, obtain resin and the waste liquid of Adsorption of Tea Polyphenols, then adopt 3 * 10
-4mol/L tartaric acid solution and 85% edible alcohol solution carry out wash-out to the resin of Adsorption of Tea Polyphenols, obtain tea-polyphenol elutriant;
Step 6, concentrate drying: tea-polyphenol elutriant is carried out to concentrated frozen and be dried, obtain tea-polyphenol finished product.
Wherein, as some embodiments of the present invention, described step 3 ultrasonic extraction condition is 20～50 ℃, extracts each 10～20min 1～3 time.
As some embodiments of the present invention, the filter residue that described step 4 separation obtains returns to step 3 again and repeats to extract.
As some embodiments of the present invention, in described step 5, waste liquid adsorbs by resin again, returns to step 3 again and repeat to extract after removal impurity;
As some embodiments of the present invention, while adding distilled water in described step 2, also can add again organic solvent.
As some embodiments of the present invention, described in step 1, drying is that tealeaves is being placed in baker, dries to ridity and reach 98% at the temperature of 70～100 ℃.
Below in conjunction with some embodiment, the present invention is further described:
Embodiment 1
As shown in Figure 1, extract the preparation technology of tea-polyphenol:
Choose high-quality tourism industry tea 1000kg, tealeaves is placed in baker, at the temperature of 70 ℃, dry to ridity and reach 98%, after oven dry, pulverize, cross 60 mesh sieves, obtain tea powder; Tea powder is placed in extraction kettle, adds 10000kg distilled water fully to mix, the oxygen with the de-distilled water of vacuum pump, then passes into pure nitrogen gas; Pass into after nitrogen, carry out ultrasonic extraction under the constant temperature of 50 ℃, extract 2 times, each 20min, obtains the tea-polyphenol solution that contains residue; By separator, the tea-polyphenol solution that contains residue is filtered, separation obtains extracting solution and filter residue, and the filter residue obtaining returns and carries out ultrasonic extraction; With the tea-polyphenol of polyamide resin adsorbing and extracting liquid, obtain resin and the waste liquid of Adsorption of Tea Polyphenols, then adopt 3 * 10
-4mol/L tartaric acid solution and 85% edible alcohol solution carry out wash-out to the resin of Adsorption of Tea Polyphenols, obtain tea-polyphenol elutriant; Tea-polyphenol elutriant is carried out to concentrated frozen and be dried, obtain tea-polyphenol finished product.
Waste liquid adsorbs by resin again, after removal impurity, returns and repeats ultrasonic extraction.
Embodiment 2
As shown in Figure 1, extract the preparation technology of tea-polyphenol:
Choose high-quality tourism industry tea 1000kg, tealeaves is placed in baker, at the temperature of 100 ℃, dry to ridity and reach 98%, after oven dry, pulverize, cross 60 mesh sieves, obtain tea powder; Tea powder is placed in extraction kettle, adds distilled water 6000kg fully to mix, the oxygen with the de-distilled water of vacuum pump, then passes into pure nitrogen gas; Pass into after nitrogen, carry out ultrasonic extraction under the constant temperature of 30 ℃, extract 3 times, each 15min, obtains the tea-polyphenol solution that contains residue; By separator, the tea-polyphenol solution that contains residue is filtered, separation obtains extracting solution and filter residue, and the filter residue obtaining returns and carries out ultrasonic extraction; With the tea-polyphenol of polyamide resin adsorbing and extracting liquid, obtain resin and the waste liquid of Adsorption of Tea Polyphenols, then adopt 3 * 10
-4mol/L tartaric acid solution and 85% edible alcohol solution carry out wash-out to the resin of Adsorption of Tea Polyphenols, obtain tea-polyphenol elutriant; Tea-polyphenol elutriant is carried out to concentrated frozen and be dried, obtain tea-polyphenol finished product.
Waste liquid adsorbs by resin again, after removal impurity, returns and repeats ultrasonic extraction.
Embodiment 3
As shown in Figure 1, extract the preparation technology of tea-polyphenol:
Choose high-quality tourism industry tea 1000kg, tealeaves is placed in baker, at the temperature of 85 ℃, dry to ridity and reach 98%, after oven dry, pulverize, cross 80 mesh sieves, obtain tea powder; Tea powder is placed in extraction kettle, adds distilled water 15000kg fully to mix, the oxygen with the de-distilled water of vacuum pump, then passes into pure nitrogen gas; Pass into after nitrogen, carry out ultrasonic extraction under the constant temperature of 40 ℃, extract 2 times, each 10min, obtains the tea-polyphenol solution that contains residue; By separator, the tea-polyphenol solution that contains residue is filtered, separation obtains extracting solution and filter residue, and the filter residue obtaining returns and carries out ultrasonic extraction; With the tea-polyphenol of polyamide resin adsorbing and extracting liquid, obtain resin and the waste liquid of Adsorption of Tea Polyphenols, then adopt 3 * 10
-4mol/L tartaric acid solution and 85% edible alcohol solution carry out wash-out to the resin of Adsorption of Tea Polyphenols, obtain tea-polyphenol elutriant; Tea-polyphenol elutriant is carried out to concentrated frozen and be dried, obtain tea-polyphenol finished product.
Waste liquid adsorbs by resin again, after removal impurity, returns and repeats ultrasonic extraction.
The tea-polyphenol finished product being prepared by above-described embodiment, and the tea-polyphenol for preparing of other embodiments of the invention, its quality meets QB2154-54 quality standard completely.See table 1:
Content's index in the tea-polyphenol finished product that table 1 the present invention prepares
Claims (6)
1. from tealeaves, extract the preparation technology of tea-polyphenol, it is characterized in that comprising the following steps:
Step 1, tealeaves pre-treatment: choose high-quality tea, for tourism industry tealeaves, pulverize after oven dry, cross 60～80 mesh sieves, obtain tea powder;
Step 2, nitrogen protection: the tea powder of step 1 is placed in extraction kettle, adds distilled water fully to mix, feed liquid mass ratio is 1:6～1:15, uses vacuum pump deoxidation, then passes into pure nitrogen gas;
Step 3, supersound extraction: pass into after nitrogen, constant temperature carries out ultrasonic extraction, obtains the tea-polyphenol solution that contains residue;
Step 4, separation: by separator, the tea-polyphenol solution that contains residue in step 3 is filtered, separation obtains extracting solution and filter residue;
Step 5, resin absorption: with the tea-polyphenol of extracting solution in polyamide resin or NKA macroporous resin adsorption step 4, obtain resin and the waste liquid of Adsorption of Tea Polyphenols, then the resin of Adsorption of Tea Polyphenols is carried out to wash-out, obtain tea-polyphenol elutriant;
Step 6, concentrate drying: tea-polyphenol elutriant is carried out to concentrated frozen and be dried, obtain tea-polyphenol finished product.
2. the preparation technology who extracts tea-polyphenol from tealeaves as claimed in claim 1, is characterized in that: described step 3 ultrasonic extraction condition is 20～50 ℃, extracts each 10～20min 1～3 time.
3. the preparation technology who extracts tea-polyphenol from tealeaves as claimed in claim 1, is characterized in that: the filter residue that described step 4 separation obtains returns to step 3 again and repeats to extract.
4. the preparation technology who extracts tea-polyphenol from tealeaves as claimed in claim 1, is characterized in that: in described step 5, waste liquid adsorbs by resin again, returns to step 3 again and repeat to extract after removal impurity.
5. the preparation technology who extracts tea-polyphenol from tealeaves as claimed in claim 1, is characterized in that: while adding distilled water in described step 2, also can add organic solvent again.
6. the preparation technology who extracts tea-polyphenol from tealeaves as claimed in claim 1, is characterized in that: described in step 1, drying is that tealeaves is being placed in baker, dries to ridity and reach 98% at the temperature of 70～100 ℃.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104186812A (en) * | 2014-09-10 | 2014-12-10 | 江苏吟春碧芽股份有限公司 | Method for processing tea polyphenol extracting raw material |
| CN104186811A (en) * | 2014-09-10 | 2014-12-10 | 江苏吟春碧芽股份有限公司 | Tea polyphenol extraction process |
| CN105498484A (en) * | 2016-01-12 | 2016-04-20 | 福州众天环保科技有限公司 | Preparation method of plant polyphenol formaldehyde catching agent |
| CN105693780A (en) * | 2014-11-25 | 2016-06-22 | 河南智晶生物科技股份有限公司 | Tea polyphenol extraction method |
| CN105712897A (en) * | 2015-01-25 | 2016-06-29 | 宜昌绿源生物技术有限公司 | Tea polyphenol extracting and recycling method |
| CN106478744A (en) * | 2016-08-26 | 2017-03-08 | 潜山县妙山茶业有限公司 | A kind of technique extracting tea polyphenols from Folium Camelliae sinensis |
| CN106914032A (en) * | 2017-02-28 | 2017-07-04 | 南京元凯生物能源环保工程有限公司 | The extraction element and its preparation technology of a kind of Tea Polyphenols |
| CN107029051A (en) * | 2016-12-09 | 2017-08-11 | 昭平县科学技术指导站 | A kind of extraction process of Tea Polyphenols in Tea |
| CN107455521A (en) * | 2017-08-16 | 2017-12-12 | 广西克鲁尼茶叶生物科技有限公司 | A kind of complex art for being used for the high efficiency extraction Tea Polyphenols from discarded tealeaves |
| CN107518112A (en) * | 2016-06-20 | 2017-12-29 | 勐海茶业有限责任公司 | A kind of method for separating Pu'er tea component |
| CN109096345A (en) * | 2018-08-16 | 2018-12-28 | 福建农林大学 | It is extracted in a kind of tealeaves and purifying tea polyphenols method |
| CN110845464A (en) * | 2019-11-21 | 2020-02-28 | 葛定军 | Extraction method of tea polyphenol |
| CN111116680A (en) * | 2020-01-03 | 2020-05-08 | 海山都(上海)生物技术有限公司 | Process for extracting and purifying high-quality tea polyphenol by using spherical polyamide resin |
| CN111184798A (en) * | 2020-02-12 | 2020-05-22 | 佛山市鼎科科技发展有限公司 | Method for purifying tea polyphenol based on column chromatography |
| CN112674190A (en) * | 2020-12-24 | 2021-04-20 | 云南省农业科学院茶叶研究所 | Method for extracting low-caffeine, no-pesticide residue and no-ester tea polyphenol from tea leaves |
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- 2014-05-08 CN CN201410190405.6A patent/CN103992359A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104186812A (en) * | 2014-09-10 | 2014-12-10 | 江苏吟春碧芽股份有限公司 | Method for processing tea polyphenol extracting raw material |
| CN104186811A (en) * | 2014-09-10 | 2014-12-10 | 江苏吟春碧芽股份有限公司 | Tea polyphenol extraction process |
| CN105693780A (en) * | 2014-11-25 | 2016-06-22 | 河南智晶生物科技股份有限公司 | Tea polyphenol extraction method |
| CN105712897A (en) * | 2015-01-25 | 2016-06-29 | 宜昌绿源生物技术有限公司 | Tea polyphenol extracting and recycling method |
| CN105498484A (en) * | 2016-01-12 | 2016-04-20 | 福州众天环保科技有限公司 | Preparation method of plant polyphenol formaldehyde catching agent |
| CN107518112A (en) * | 2016-06-20 | 2017-12-29 | 勐海茶业有限责任公司 | A kind of method for separating Pu'er tea component |
| CN106478744A (en) * | 2016-08-26 | 2017-03-08 | 潜山县妙山茶业有限公司 | A kind of technique extracting tea polyphenols from Folium Camelliae sinensis |
| CN107029051A (en) * | 2016-12-09 | 2017-08-11 | 昭平县科学技术指导站 | A kind of extraction process of Tea Polyphenols in Tea |
| CN106914032A (en) * | 2017-02-28 | 2017-07-04 | 南京元凯生物能源环保工程有限公司 | The extraction element and its preparation technology of a kind of Tea Polyphenols |
| CN107455521A (en) * | 2017-08-16 | 2017-12-12 | 广西克鲁尼茶叶生物科技有限公司 | A kind of complex art for being used for the high efficiency extraction Tea Polyphenols from discarded tealeaves |
| CN109096345A (en) * | 2018-08-16 | 2018-12-28 | 福建农林大学 | It is extracted in a kind of tealeaves and purifying tea polyphenols method |
| CN110845464A (en) * | 2019-11-21 | 2020-02-28 | 葛定军 | Extraction method of tea polyphenol |
| CN111116680A (en) * | 2020-01-03 | 2020-05-08 | 海山都(上海)生物技术有限公司 | Process for extracting and purifying high-quality tea polyphenol by using spherical polyamide resin |
| CN111184798A (en) * | 2020-02-12 | 2020-05-22 | 佛山市鼎科科技发展有限公司 | Method for purifying tea polyphenol based on column chromatography |
| CN112674190A (en) * | 2020-12-24 | 2021-04-20 | 云南省农业科学院茶叶研究所 | Method for extracting low-caffeine, no-pesticide residue and no-ester tea polyphenol from tea leaves |
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Application publication date: 20140820 |