CN111825673A - Method for extracting tea polysaccharide and caffeine from autumn and winter tea leaves - Google Patents
Method for extracting tea polysaccharide and caffeine from autumn and winter tea leaves Download PDFInfo
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- CN111825673A CN111825673A CN202010636490.XA CN202010636490A CN111825673A CN 111825673 A CN111825673 A CN 111825673A CN 202010636490 A CN202010636490 A CN 202010636490A CN 111825673 A CN111825673 A CN 111825673A
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 49
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- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229960001948 caffeine Drugs 0.000 title claims abstract description 31
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 21
- 241001122767 Theaceae Species 0.000 title claims 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 86
- 238000001914 filtration Methods 0.000 claims abstract description 47
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D473/00—Heterocyclic compounds containing purine ring systems
- C07D473/02—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6
- C07D473/04—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms
- C07D473/06—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3
- C07D473/12—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3 with methyl radicals in positions 1, 3, and 7, e.g. caffeine
-
- 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
Abstract
The invention belongs to the technical field of deep processing of tea raw materials, and particularly relates to a method for extracting tea polysaccharide and caffeine from autumn and winter tea. The invention comprises the following steps: A. a pretreatment stage: (1) air-drying fresh tea raw materials into coarse powder; (2) hot water circulation ultrasonic treatment; (3) coarse filtration and fine filtration are carried out; (4) concentrating under reduced pressure to obtain filtrate; (5) precipitating the impure protein by using ethanol; B. extracting tea polysaccharide: (6) centrifuging/filtering to obtain crude polysaccharide; (7) dissolving the precipitate in hot water, removing protein and decolorizing; (8) centrifuging/filtering, and precipitating with ethanol; (9) (ii) centrifuged/filtered fine polysaccharide; (10) drying under reduced pressure to obtain dried tea polysaccharide. C. Extracting caffeine: (11) decoloring the filtrate obtained in the step (6), and centrifuging/filtering; (12) concentrating the filtrate to obtain crystals; (13) washing and drying the crystal; (14) decompressing and sublimating to obtain pure caffeine. The invention can improve the comprehensive utilization rate and the utilization value of the autumn and winter tea tree resource.
Description
Technical Field
The invention belongs to the technical field of tea deep processing, and particularly relates to a method for extracting tea polysaccharide and caffeine from autumn and winter tea (raw materials).
Background
Xinyang Maojian tea is a famous and excellent tea product in Xinyang areas of Henan province, raw materials of the Xinyang Maojian tea mainly utilize fresh bud tips of locally produced tea trees, but in the whole growth process of the tea trees, the yield of the bud tips is low, the picking period is short, and the supply of the raw materials is short. Meanwhile, a large amount of fresh tea leaves, particularly tea leaves trimmed in autumn and winter, can be left in a tea garden, so that resource waste is caused, and the sustainable utilization of tea tree resources is seriously restricted.
The tea mainly contains tea polysaccharide as a bioactive component, and the tea polysaccharide plays a unique role in reducing blood sugar, resisting fatigue, resisting oxidation, resisting tumor cells and the like and can be used for developing functional foods. The caffeine extracted from the tea leaves has the effects of removing fatigue and exciting nerves when being drunk in a proper amount, is clinically used for treating neurasthenia and coma resuscitation, and can be used for developing raw material medicines. The content types and contents of the tea leaves in the period from autumn to snowy are obviously different from other seasons, for example, the content of polysaccharide in the tea leaves in the season accounts for about 16-21% of the dry weight of the tea leaves, the content of caffeine accounts for about 2-3% of the dry weight of the tea leaves, and the contents of tea polyphenol, amino acid, theophylline, theobromine and the like are reduced, so that the tea leaves are not beneficial to making high-grade drinking tea, but are beneficial to extracting tea polysaccharide and caffeine. The tea leaves in autumn and winter have no insect damage, no pesticide is used, and the residue is low. Can realize mechanical pruning and leaf harvesting, is favorable for the germination of spring tea in the next year, has consistent germination and is also favorable for the picking of spring tea.
Disclosure of Invention
The invention aims to provide a method for extracting tea polysaccharide and caffeine from autumn and winter tea leaves, which aims to solve the technical problems in the prior art.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the method takes unprocessed tea leaves in autumn and winter in Xinyang areas as raw materials, improves the dissolution rate of the dissolved substances and shortens the extraction time by a cyclic ultrasonic-assisted hot water extraction method in a pretreatment stage. In the tea polysaccharide extraction process, the organic solvent only relates to ethanol, and the recycling of ethanol and water is increased in the extraction process. In the caffeine extraction process, the invention adopts a nanofiltration concentration series reverse osmosis technology to replace the traditional decompression concentration process, thereby realizing energy saving and high efficiency, and the obtained RO water can provide high-purity water for the whole production process.
Specifically, the technical scheme of the invention is as follows:
a process for extracting tea polysaccharides and caffeine from autumn and winter season tea leaves (for convenience of description the invention is referred to collectively as tea leaves, which are essentially raw tea leaves, i.e., tea leaf material, the following) comprising the steps of:
(1) pretreatment: air-drying fresh autumn and winter tea leaves collected from 10 middle ten days to 12 last ten days, pulverizing into raw materials with the size of 0.1-5mm, adding water with the temperature of 90-100 ℃ according to the liquid-solid ratio of 15-20:1, filtering out tea leaf residues to obtain filtrate 1, and extracting tea polysaccharide and caffeine from the tea coarse powder by using a cyclic ultrasonic method, wherein the ultrasonic frequency in the cyclic ultrasonic method is 45-70kHz, the output power is 60-90%, and the ultrasonic treatment time is 20-70 min; performing solid-liquid separation by plate-and-frame filter pressing, concentrating the obtained filtrate 1 at 40-50 deg.C under 0.09-0.1MPa, adding 95-100% ethanol into the concentrated solution 1 to make ethanol concentration reach 75-80%; and (3) carrying out solid-liquid separation on the liquid after alcohol precipitation by adopting a centrifugal or filtration mode, wherein the obtained precipitate or retentate is the crude tea polysaccharide.
(2) Preparing high-purity tea polysaccharide: dissolving the crude tea polysaccharide obtained in step (1) with hot water at 95-100 deg.C, adding 20% trichloroacetic acid to 6% precipitate impurity protein, decolorizing with 4-6 mesh granular activated carbon, filtering to obtain filtrate 4, and adding anhydrous ethanol into filtrate 4 until ethanol concentration is 75-80%; precipitating tea polysaccharide again, filtering, and drying under reduced pressure to obtain high-purity tea polysaccharide with content of not less than 90%.
(3) Extracting caffeine: carrying out solid-liquid separation on the liquid subjected to alcohol precipitation in the step (1) by adopting a centrifugation or filtration mode to obtain a filtrate 2; distilling under reduced pressure to recover ethanol, adding 20% trichloroacetic acid into the obtained residual liquid until the concentration is 6% to precipitate protein impurities, decolorizing with granular activated carbon, filtering with a grading membrane to obtain filtrate 3, concentrating by nanofiltration to obtain concentrated solution 2, and passing the filtered clear liquid through a reverse osmosis device (conventional, commercially available equipment) to obtain high-purity RO water; cooling the concentrated solution 2 to crystallize to obtain coarse caffeine crystal; then carrying out decompression sublimation at the temperature of 100-105 ℃ to obtain the caffeine pure product with the purity of more than or equal to 99 percent.
The leftovers of the invention after extracting tea polysaccharide and caffeine, such as tea filter residue, can be used for producing animal feed or organic fertilizer by adopting a microorganism solid fermentation method.
The invention has the beneficial effects that:
(1) the utilization rate of tea products for making drinking tea from tea leaves in autumn and winter in China is low, and the main reason is that the tea leaves in this period have lower content of main components as drinking tea and are not suitable for making high-grade drinking tea. However, the tea polysaccharide and caffeine content in the raw material tea leaves of the tea plant in this period is significantly higher than in the other periods. In the practical production, the tea leaves in the period are mainly used as the green-clearing pruning and rotten tea garden. Xinyang is a key tea area in China, tea resources in autumn and winter are rich, and the process can be used for the perpetual utilization of the tea resources in autumn and winter, and especially lays a technical foundation for extracting tea polysaccharide and caffeine from the tea resources.
(2) The process of the invention adopts a membrane separation technology, and has the characteristics of energy conservation, environmental protection and high-efficiency production.
(3) The process of the invention establishes 2 recycling links, one is the recycling of ethanol, the other is the discharge liquid after nanofiltration concentration, and the high-purity RO water can be prepared after the discharge liquid passes through a reverse osmosis device.
Drawings
FIG. 1: technical route diagrams of the present invention.
Detailed Description
Example 1
(1) A pretreatment stage: leaching by using a TGCXN-2.5B energy-gathering type ultrasonic circulation extractor which is produced by Beijing Honghong biotech GmbH. Pouring hot water of about 95 ℃ into an extraction tank of 1.5L, starting a stirring circulation system, adding 100g of coarse tea powder (with the particle size of 0.1-5mm) under stirring, uniformly mixing, and starting a temperature control system of an energy-gathering ultrasonic circulation extraction machine to ensure that the temperature in the extraction tank is not lower than 90 ℃. Starting an ultrasonic generator, and carrying out ultrasonic extraction under the conditions that the ultrasonic power is 60%, the ultrasonic working time is 4s, the working interval time is 3s, the whole course time is 20min and the temperature is 95 ℃. After the ultrasonic extraction is finished, discharging, carrying out rough filtration by using 6-8 layers of gauze, carrying out rough filtration on rough filtrate by using slow filter paper to obtain filtrate 1, suspending filter residues by using 1.0L hot water at about 95 ℃, putting the filter residues into an extraction tank, repeatedly extracting for 10min according to the ultrasonic extraction conditions and steps, carrying out solid-liquid separation again, carrying out rough filtration and fine filtration, and combining the obtained fine filtrate into the filtrate 1. Concentrating the obtained filtrate 1 under reduced pressure to 10-15% of original volume, adding 95% ethanol or anhydrous ethanol until the final concentration of ethanol is 75-80%, and performing solid-liquid separation on the liquid after ethanol precipitation to obtain precipitate or retentate, which is crude tea polysaccharide.
(2) Preparing high-purity tea polysaccharide: dissolving 100mL of crude tea polysaccharide obtained in the step (1) by using hot water at the temperature of 95-DEG C and 100 ℃ in a centrifugal or filtering mode, adding trichloroacetic acid to 6% under stirring to precipitate protein, adding a proper amount of 4-6-mesh granular activated carbon after 15min, slowly stirring to enable the granular activated carbon to be fully suspended in liquid, standing for 20-30min, performing solid-liquid separation again, adding absolute ethyl alcohol into the obtained filtrate 4, concentrating until the volume concentration of the ethyl alcohol is 75-80%, precipitating the tea polysaccharide, filtering and separating, and drying the retentate under reduced pressure to obtain a high-purity dry tea polysaccharide product.
(3) And (3) preparing caffeine: carrying out solid-liquid separation on the liquid after alcohol precipitation in the step (1) by adopting a centrifugal or filtering mode to obtain a filtrate 2, recovering ethanol under the condition of reduced pressure distillation, removing ethanol from the filtrate 2 to obtain a residual liquid, adding trichloroacetic acid under the stirring condition until the final concentration reaches 6% to precipitate protein impurities in the residual liquid, adding a proper amount of 4-6 mesh granular activated carbon after 15min, slowly stirring to enable the granular activated carbon to be fully suspended in the residual liquid, standing for 20-30min, carrying out solid-liquid separation by adopting membrane separation technologies of different filtering stages (such as nylon membranes, phi 5 mu m/phi 2 mu m) to obtain a filtrate 3, carrying out nanofiltration concentration to obtain a concentrated solution 2, and preparing high-purity RO water by filtering a clear solution through a reverse osmosis device for recycling. And cooling and crystallizing the concentrated solution 2, washing crystals, drying, and then sublimating under reduced pressure at the temperature of 100-105 ℃ to obtain the high-purity caffeine (not less than 99%).
Example 2
The specific process flow is as follows:
(1) a pretreatment stage: leaching by using a TGCXN-20B energy-gathering type ultrasonic circulation extractor of Beijing Honghong biotechnology GmbH. Adding hot water 15L at about 95 deg.C into extraction tank, starting stirring circulation system, adding pulverized coarse tea powder (particle size of 0.1-5mm) 1.0kg under stirring, mixing, starting temperature control system, and maintaining the temperature in extraction tank at not lower than 90 deg.C. Starting an ultrasonic generator, and carrying out ultrasonic leaching at the temperature of 95 ℃ under the conditions of ultrasonic power of 70%, ultrasonic working time of 4s, working interval time of 3s and whole course time of 35 min. After the ultrasonic extraction is finished, discharging, and filtering the obtained liquid by using a non-woven filter cloth with 100 meshes for coarse filtration by using a ceramic membrane (phi 60-120 mu m) to obtain a filtrate 1; suspending the filter residue with 10L of hot water of 95 deg.C, placing into an extraction tank, repeatedly performing ultrasonic extraction for 10min according to the above ultrasonic treatment standard, performing solid-liquid separation again, coarse filtering, fine filtering, and mixing the liquid to obtain filtrate 1. Concentrating the obtained filtrate 1 under reduced pressure to 10-15% of original volume to obtain concentrated solution 1, adding 95% ethanol or anhydrous ethanol until the final concentration of ethanol volume ratio reaches 75-80%, centrifuging or filtering to perform solid-liquid separation on the concentrated solution 1 after ethanol precipitation to obtain precipitate or retentate, which is crude tea polysaccharide.
(2) Preparing high-purity tea polysaccharide: dissolving crude tea polysaccharide with 1.0L of hot water of 95-100 ℃, adding trichloroacetic acid under stirring until the concentration is 6% to precipitate protein impurities, adding a proper amount of 4-6 mesh granular activated carbon after 15min, slowly stirring to fully suspend the granular activated carbon, standing for 25-35min, performing solid-liquid separation, adding absolute ethyl alcohol into the obtained filtrate 4 until the volume ratio concentration of the ethanol is 75% -80%, precipitating the tea polysaccharide, filtering and separating, and drying the precipitate under reduced pressure to obtain the high-purity dry tea polysaccharide.
(3) Extracting caffeine: carrying out solid-liquid separation on the concentrated solution 1 subjected to alcohol precipitation in the step (1) by adopting a centrifugation or filtration mode to obtain a filtrate 2, carrying out reduced pressure distillation on the filtrate 2 to recover ethanol to obtain a residual solution, adding trichloroacetic acid to the concentration of 6% under the stirring condition to precipitate protein impurities, adding a proper amount of 4-6 mesh granular activated carbon to decolor the residual solution after 15min, slowly stirring to enable the granular activated carbon to be fully suspended in the residual solution, standing for 25-35min, carrying out coarse filtration by adopting 100-mesh non-woven filter cloth, then carrying out secondary filtration by using a ceramic membrane (phi 60-120 mu m) to obtain a filtrate 3, carrying out nanofiltration to concentrate the filtrate 3 to obtain a concentrated solution 2, and preparing high-purity RO water from the filtered clear solution by using a. And cooling and crystallizing the concentrated solution 2, washing crystals, drying, and sublimating under reduced pressure at the temperature of 100-105 ℃ to obtain the high-purity caffeine (not less than 99%).
Example 3
(1) A pretreatment stage: leaching by using a TGCXN-200B energy-gathering type ultrasonic circulation extractor which is produced by Beijing Honghong biotechnology GmbH. Adding hot water 150L at 95 deg.C into extraction tank, starting stirring circulation system, adding 10kg of coarse tea powder (particle size of 0.1-5mm) under stirring, mixing, and starting temperature control system to make the temperature in extraction tank not lower than 90 deg.C. Starting an ultrasonic generator (whether the TGCXN-200B energy-gathering type ultrasonic circulation extractor mentioned above is used, whether the extractor carries the ultrasonic generator or needs to be additionally provided with an ultrasonic generator device), carrying out ultrasonic extraction at the ultrasonic power of 85 percent, the ultrasonic working time of 4s, the working interval time of 3s and the whole working time of 70min, and carrying out ultrasonic extraction at the temperature of 95 ℃. Discharging the material liquid after the ultrasonic extraction is finished, performing coarse filtration by using a plate-and-frame filter press (sieving with a 100-mesh sieve), and filtering the coarse filtrate by using a ceramic membrane (phi 60-120 mu m) to obtain a filtrate 1; suspending the residue with 100L of hot water of 95 deg.C, placing into an extraction tank, repeatedly performing ultrasonic extraction for 40min, performing solid-liquid separation again, coarse filtering, fine filtering, and mixing the filtrate 1. Concentrating the filtrate 1 under reduced pressure to original volume of 15-20% to obtain concentrated solution 1, adding 95% ethanol or anhydrous ethanol until the final concentration of ethanol in the concentrated solution 1 is 75-80%, centrifuging or filtering to perform solid-liquid separation on the concentrated solution 1 after ethanol precipitation to obtain precipitate or retentate as crude tea polysaccharide.
(2) Preparing high-purity tea polysaccharide: and (3) carrying out solid-liquid separation on the liquid precipitated in the step (1) by adopting a centrifugal or filtration mode, wherein the obtained precipitate or retentate is the crude tea polysaccharide. Dissolving crude tea polysaccharide in 10L of 95-100 ℃ hot water, adding trichloroacetic acid under stirring until the concentration is 6% to precipitate protein impurities, adding the crude tea polysaccharide solution into a granular activated carbon filter (4-6 meshes) for decoloring after 20min, standing for 25-35min, filtering the decolored liquid by a ceramic membrane (phi 60-120 mu m), adding absolute ethyl alcohol into the obtained filtrate 4 until the volume concentration of the ethyl alcohol is 75% -80%, precipitating to obtain tea polysaccharide, centrifuging or filtering to separate precipitates, and drying the precipitates under reduced pressure to obtain a high-purity dried tea polysaccharide product.
(3) Extracting caffeine: and (2) carrying out solid-liquid separation on the concentrated solution 1 subjected to alcohol precipitation in the step (1) by adopting a centrifugation or filtration mode to obtain a filtrate 2, carrying out reduced pressure distillation on the filtrate 2 to recover ethanol to obtain a residual solution, adding trichloroacetic acid to the residual solution until the concentration of trichloroacetic acid is 6% under the stirring condition to precipitate protein impurities, adding the residual solution after the protein impurities are precipitated into a particle activated carbon filter (4-6 meshes) for decolorization after 20min, standing for 25-35min, filtering the decolorized liquid by using a ceramic membrane (phi 60-120 mu m) to obtain a filtrate 3, carrying out nanofiltration concentration on the filtrate 3 to obtain a concentrated solution 2, and preparing high-purity RO water by using a reverse osmosis device to obtain the high-. And cooling and crystallizing the concentrated solution 2, washing crystals, drying, and sublimating under reduced pressure at the temperature of 100-105 ℃ to obtain the high-purity caffeine (not less than 99%).
Claims (2)
1. A method for extracting tea polysaccharide and caffeine from tea leaves in autumn and winter is characterized by comprising the following steps:
(1) pretreatment: air-drying fresh autumn and winter tea leaves collected from 10 middle ten days to 12 last ten days of the month, then crushing the tea leaves to 0.1-5mm, adding water with the temperature of 95-100 ℃ according to the liquid-solid ratio of 15-20:1, filtering out tea leaf residues to obtain filtrate 1, and extracting tea polysaccharide and caffeine in the tea coarse powder by using a circulating ultrasonic method, wherein the ultrasonic frequency in the circulating ultrasonic method is 45-70kHz, the output power is 60-90%, and the ultrasonic time is 20-70 min; performing solid-liquid separation by adopting plate and frame filter pressing, performing reduced pressure concentration on the obtained filtrate 1 at 40-50 ℃ under the condition of 0.09-0.1MPa, adding 95-100% of ethanol into the concentrated solution 1 to enable the final concentration of the ethanol to be 75-80%, performing solid-liquid separation on the liquid after ethanol precipitation by adopting a centrifugal or filtration mode, and obtaining precipitate or retentate, namely crude tea polysaccharide;
(2) preparing high-purity tea polysaccharide: dissolving the crude tea polysaccharide obtained in step (1) with hot water at 95-100 deg.C, adding 20% trichloroacetic acid to 6% to precipitate protein impurities, decolorizing with 4-6 mesh granular activated carbon, filtering, and adding anhydrous ethanol into filtrate 4 until the volume concentration of ethanol is 75-80%; precipitating tea polysaccharide again, filtering, and drying under reduced pressure to obtain high-purity tea polysaccharide with content of more than or equal to 90%;
(3) extracting caffeine: carrying out solid-liquid separation on the liquid subjected to alcohol precipitation in the step (1) by adopting a centrifugal or filtering mode to obtain a filtrate 2, carrying out reduced pressure distillation to recover ethanol, adding 20% trichloroacetic acid into the obtained residual liquid until the concentration of trichloroacetic acid is 6% to precipitate protein impurities, decoloring by using granular activated carbon, filtering by using a grading membrane to obtain a filtrate 3, carrying out nanofiltration concentration to obtain a concentrated solution 2, and filtering the waste liquid to obtain high-purity water by using a reverse osmosis device; cooling the concentrated solution 2 to crystallize to obtain coarse caffeine crystal, and sublimating at 100-105 deg.C under reduced pressure to obtain pure caffeine product with purity not lower than 99%.
2. The method for extracting tea polysaccharides and caffeine from autumn winter tea leaves as claimed in claim 1, wherein: and recovering ethanol in the filtrate 2 by adopting a reduced pressure distillation mode, or concentrating the filtrate 3 by adopting nanofiltration to obtain a concentrated solution 2, and simultaneously filtering waste liquid to obtain high-purity RO water by using a reverse osmosis device.
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| CN112877482A (en) * | 2020-12-30 | 2021-06-01 | 江西神州通油茶科技有限公司 | Method for extracting xylooligosaccharide from camellia oleifera shells |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699586A (en) * | 2005-04-29 | 2005-11-23 | 西北大学 | Process for extracting tea polyphenol, caffeine as a byproduct thereof and tea polysaccharide from tea |
| CN1837201A (en) * | 2006-02-21 | 2006-09-27 | 张守政 | Process for extracting tea polyphenol, theanine, tea polysaccharide and tea pigment from tea |
| CN105399741A (en) * | 2015-11-30 | 2016-03-16 | 云南茶农生物产业有限责任公司 | Method for extracting high-purity caffeine from tea leaves |
| CN109170068A (en) * | 2018-07-16 | 2019-01-11 | 云南茶农生物产业有限责任公司 | A kind of method of UF membrane removing caffeine |
| CN109251252A (en) * | 2018-07-25 | 2019-01-22 | 云南茶农生物产业有限责任公司 | A kind of technique that membrane separation technique combines cooling precipitation method to prepare tea polysaccharide, tea polyphenols, caffeine and theanine |
-
2020
- 2020-07-04 CN CN202010636490.XA patent/CN111825673A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1699586A (en) * | 2005-04-29 | 2005-11-23 | 西北大学 | Process for extracting tea polyphenol, caffeine as a byproduct thereof and tea polysaccharide from tea |
| CN1837201A (en) * | 2006-02-21 | 2006-09-27 | 张守政 | Process for extracting tea polyphenol, theanine, tea polysaccharide and tea pigment from tea |
| CN105399741A (en) * | 2015-11-30 | 2016-03-16 | 云南茶农生物产业有限责任公司 | Method for extracting high-purity caffeine from tea leaves |
| CN109170068A (en) * | 2018-07-16 | 2019-01-11 | 云南茶农生物产业有限责任公司 | A kind of method of UF membrane removing caffeine |
| CN109251252A (en) * | 2018-07-25 | 2019-01-22 | 云南茶农生物产业有限责任公司 | A kind of technique that membrane separation technique combines cooling precipitation method to prepare tea polysaccharide, tea polyphenols, caffeine and theanine |
Non-Patent Citations (6)
| Title |
|---|
| 李春雷等: "茶多糖提取分离工艺综述", 《中国茶叶加工》 * |
| 王瑞芳等: "茶叶中有效成分的开发利用进展", 《亚热带农业研究》 * |
| 葛艳: "夏秋绿茶中茶氨酸的提取分离纯化及对肠道微生态的影响", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
| 贺佳等: "茶叶有效成分综合提取分离生产工艺", 《江苏农业科学》 * |
| 远凌威等: "几种信阳毛尖茶的化学成分研究", 《信阳师范学院学报》 * |
| 邹锋扬等: "膜过滤技术在茶叶深加工中的应用研究进展", 《经济发展方式转变与自主创新——第十二届中国科学技术协会年会（第二卷）》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112877482A (en) * | 2020-12-30 | 2021-06-01 | 江西神州通油茶科技有限公司 | Method for extracting xylooligosaccharide from camellia oleifera shells |
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