CN101343270B - Method for extracting tea polyphenol and theine from tea simultaneously - Google Patents
Method for extracting tea polyphenol and theine from tea simultaneously Download PDFInfo
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- CN101343270B CN101343270B CN2008101070665A CN200810107066A CN101343270B CN 101343270 B CN101343270 B CN 101343270B CN 2008101070665 A CN2008101070665 A CN 2008101070665A CN 200810107066 A CN200810107066 A CN 200810107066A CN 101343270 B CN101343270 B CN 101343270B
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- ethyl acetate
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- tealeaves
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Abstract
Disclosed is a method for extracting tea polyphenol and theine from tea leaves, which is characterized in that the method simultaneously acquires tea polyphenol and theine through steps of leaching with boiled water, precipitation filtration, extraction, drying, etc., the method has the technical effects that: 1. the theine is transferred into an organic solvent phase by utilizing the feature that the theine is freely soluble in ethyl acetate and the impurity of cellulose, a desiccant is added for removing the excessive moisture, then the preparation of a solid product is implemented; 2. the tea polyphenol is released from precipitation, the tea polyphenol is transferred into the organic solvent phase for removing the impurity and carrying out the concentration and then preparing the solid product; and 3. the method has advantages of low equipment requirements, mild reaction conditions, low cost, safe and reliable production, high product purity and high yield.
Description
Technical field
The present invention relates to a kind of method of extracting tea-polyphenol and trimethyl-xanthine, relate in particular to a kind of method of from tealeaves, extracting tea-polyphenol and trimethyl-xanthine simultaneously.
Background technology
Modern scientific research shows, tea-polyphenol can be removed human free radical and improve immunizing power in the tealeaves, has medical health care functions such as anti-oxidant, anti-ageing, radioprotective, anticancer change, and successfully is applied to medicine, healthcare products, grease and food service industry.Trimethyl-xanthine has effects such as cardiac stimulus, excited cerebral nerve and diuresis, therefore can be used as central nervous stimulant.From tealeaves, extract the method for tea-polyphenol, according to the domestic and international Searches of Patent Literature, can reduce four classes at present: i.e. solvent extraction method, ion precipitation method, resin adsorption method and supercritical carbon dioxide extraction method, the present all shortcomings of various degrees of aforesaid method: low as ion precipitation method yield, corresponding cost height; The product of solvent extration exists organic solvent residue; Resin adsorption method technology is loaded down with trivial details, and cost is also high, is difficult to large-scale production, and the supercritical carbon dioxide extraction method still lacks the maturity of technology and reliability at present, awaits further Depth Study.
Summary of the invention
The object of the present invention is to provide a kind of method of extracting tea-polyphenol and trimethyl-xanthine from tealeaves simultaneously, this method required equipment is few, the reaction conditions gentleness, and the low production safety of cost is reliable, product purity height, productive rate height.
The present invention is achieved like this, and it is characterized in that the processing method step is:
With hot water boiling tealeaves under condition of stirring, add metal-salt and alkali while hot, adjust about pH=8, filter, collect filtrate and filter residue respectively, the treatment process of filtrate has two kinds: a kind of is to add the organic solvent extract extraction, repeatable operation several times after, get the organic solvent layer rotary evaporation and reclaim organic solvent, concentrated solution vacuum-drying or use Nitrogen evaporator are blown away organic solvent, get solid phase prod and be trimethyl-xanthine, another kind is to add organic solvent extraction, adds siccative in the organic phase again and absorbs moisture, put into the electrically heated cover, adjust temperature at 180 ℃, carefully add thermal distillation, evaporate fully up to organic solvent, the residue crystal is trimethyl-xanthine, filter residue soaks with mineral acid, treat filter residue dissolving after, add organic solvent extraction, repeatable operation several times after, get the organic solvent layer rotary evaporation and reclaim organic solvent, concentrated solution vacuum-drying or use Nitrogen evaporator are blown away organic solvent, get solid phase prod and are tea-polyphenol.
In the method for the present invention, it is characterized in that metal-salt can be directly adds with solid state, add after also can being mixed with the aqueous solution that the effect of metal-salt mainly is the tea-polyphenol in the precipitation extracting solution, can select AgCl, HgCl
2, Pb (CH
3COO)
2, Zn (CH
3COO)
2
In the method for the present invention, what it is characterized in that the evaporating solvent use is rotary evaporation, under the state of low pressure even vacuum, removes most of solvent under lower temperature, obtains concentrated solution, is convenient to subsequent disposal, and solvent also can access repeated use.
In the method for the present invention, it is characterized in that the method that extraction liquid obtains solid product is that vacuum-drying or nitrogen blow, can both effectively remove organic solvent.
Technique effect of the present invention is: 1, utilize tea-polyphenol and metal-salt easily to generate sedimentary characteristics, tea-polyphenol is separated with trimethyl-xanthine, extract respectively; 2, utilize trimethyl-xanthine to be soluble in ethyl acetate and impurity Mierocrystalline cellulose, the insoluble characteristics of protein, with trimethyl-xanthine transfer to organic solvent mutually in, thereby further remove impurity, add siccative and remove redundant moisture, carry out the solid product preparation again; 3, utilize tea-polyphenol and metal salt precipitate to be dissolved in the characteristics of mineral acid, tea-polyphenol is discharged from precipitation, utilizes tea-polyphenol to be soluble in the characteristics of ethyl acetate again, with tea-polyphenol transfer to organic solvent mutually in, remove impurity, concentrate, carry out the solid product preparation again; 4, working method is easy, uses rotary evaporation and vacuum-drying or Nitrogen evaporator just can finish the preparation of two kinds of solid products, and required equipment is few, the reaction conditions gentleness, and cost is low, and production safety is reliable, product purity height, productive rate height.
Embodiment
Embodiment one:
Get 300g tealeaves and water with 1: 7 mixed, after decocting 50min, filter with 400 order filter clothes, add the 75g zinc acetate in the filtrate, send into press filtration in the pressure filter after the stirring, add the NaOH solid in the filtrate again, adjust pH=8.2, agitation and filtration, further removal of impurities, liquid after the removal of impurities, with 40% ethyl acetate extraction of filtrate volume for the first time, vibration 5min leaves standstill the 10min layering, separate the upper strata ethyl acetate layer, lower floor's aqueous phase solution adds 35% ethyl acetate extraction twice of its volume, and 30% ethyl acetate of last water phase volume extracts three times again, merges the organic phase that extracts for six times, the anhydrous magnesium sulfate solid drying of adding about 5% is saturated until the anhydrous magnesium sulfate suction.Water reclaims, and wherein contains a small amount of trimethyl-xanthine, and can be used for next time, tealeaves extracts.Air distillation removes solvent, when quantity of solvent is considerably less, uses the little fire heating of low temperature (outside temperature is lower than 80 ℃) instead, all volatilizees up to solvent, obtains white, needle-shaped crystals.The ethyl acetate that distills reclaims after condensation, wherein contains a small amount of trimethyl-xanthine, can be used for extracting next time.
Merge the precipitation filter residue that adding zinc acetate and sodium hydrate solid after-filtration come out, the hydrochloric acid soln that slowly adds 2mol/L, slowly stir and dissolve fully until filter residue, equal-volume adds ethyl acetate, vibration 5min leaves standstill the 10min layering, separates the upper strata ethyl acetate layer, lower layer of water continues to add the equal-volume ethyl acetate mutually, extracting twice repeatedly merges the organic phase rotary evaporation of three extractions, adjusts vaporization temperature about 70 ℃, be convenient to the ethyl acetate volatilization, about rotary evaporation 0.5 hour, concentrate, carry out nitrogen again and blow until organic phase, blow away ethyl acetate, obtain the tea-polyphenol solid.Contain a small amount of tea-polyphenol in the ethyl acetate that rotary evaporation reclaims, can be used for extracting next time.Water reclaims, and wherein contains a small amount of tea-polyphenol, and can be used for next time, tealeaves extracts.
The tealeaves hot-water soak that filters out is filtered with filter cloth and is pressed dry triplicate.Merge the water that produces in this filtrate and the two kinds of extraction processes, join down batch tealeaves and be used for decocting.
Embodiment two:
Get 300g tealeaves and water with 1: 6 mixed, after decocting 20min, filter with 400 order filter clothes, adding mass concentration in the filtrate is 10% zinc acetate aqueous solution, the volume of zinc acetate aqueous solution accounts for filtrate volume about 30% (containing the about 50g of zinc acetate solid), send into press filtration in the pressure filter after the stirring, add mass concentration in the filtrate again and be 10% the NaOH aqueous solution, adjust pH=8, agitation and filtration, further removal of impurities, liquid after the removal of impurities is used equal volume of ethyl acetate, separates upper organic phase, lower floor's water is used equal volume of ethyl acetate again, twice of repeatable operation.Water reclaims, and wherein contains a small amount of trimethyl-xanthine, and can be used for next time, tealeaves extracts.The organic phase of three extractions is carried out rotary evaporation after merging, and adjusts temperature at 70 ℃, and rotary evaporation concentrated until organic phase about 0.5 hour, carried out vacuum-drying again, and vacuum tightness can reach-0.1Mpa, dry about 1 hour, can obtain the trimethyl-xanthine solid.
Merge the precipitation filter residue that adding zinc acetate and sodium hydrate solid after-filtration come out, the hydrochloric acid soln that slowly adds 2mol/L, slowly stir and dissolve fully until filter residue, equal-volume adds ethyl acetate, vibration 5min leaves standstill the 10min layering, separates the upper strata ethyl acetate layer, lower layer of water continues to add the equal-volume ethyl acetate mutually, extracting twice repeatedly merges the organic phase rotary evaporation of three extractions, adjusts vaporization temperature about 70 ℃, be convenient to the ethyl acetate volatilization, about rotary evaporation 0.5 hour, concentrate, carry out nitrogen again and blow until organic phase, blow away ethyl acetate, obtain the tea-polyphenol solid.Contain a small amount of tea-polyphenol in the ethyl acetate that rotary evaporation reclaims, can be used for extracting next time.Water reclaims, and wherein contains a small amount of tea-polyphenol, and can be used for next time, tealeaves extracts.
The tealeaves hot-water soak that filters out is filtered with filter cloth and is pressed dry triplicate.Merge the water that produces in this filtrate and the two kinds of extraction processes, join down batch tealeaves and be used for decocting.
Claims (1)
1. method of from tealeaves, extracting tea-polyphenol and trimethyl-xanthine simultaneously, it is characterized in that: get 300g tealeaves and water with 1: 7 mixed, after decocting 50min, filter with 400 order filter clothes, add the 75g zinc acetate in the filtrate, send into press filtration in the pressure filter after the stirring, add the NaOH solid in the filtrate again, adjust pH=8.2, agitation and filtration, further removal of impurities, the liquid after the removal of impurities, with 40% ethyl acetate extraction of filtrate volume for the first time, vibration 5min, leave standstill the 10min layering, separate the upper strata ethyl acetate layer, lower floor's aqueous phase solution adds twice of 35% the ethyl acetate extraction of its volume, 30% of the water phase volume ethyl acetate extracts three times more at last, the organic phase that merges six extractions, the anhydrous magnesium sulfate solid drying of adding 5% is saturated until the anhydrous magnesium sulfate suction; Water reclaims, and wherein contains a small amount of trimethyl-xanthine, and can be used for next time, tealeaves extracts; Air distillation removes solvent, when quantity of solvent is considerably less, uses the little fire heating of low temperature instead, and its outside temperature is lower than 80 ℃, all volatilizees up to solvent, obtains white, needle-shaped crystals; The ethyl acetate that distills reclaims after condensation, wherein contains a small amount of trimethyl-xanthine, can be used for extracting next time; Merge the precipitation filter residue that adding zinc acetate and sodium hydrate solid after-filtration come out, the hydrochloric acid soln that slowly adds 2mol/L, slowly stir and dissolve fully until filter residue, equal-volume adds ethyl acetate, vibration 5min leaves standstill the 10min layering, separates the upper strata ethyl acetate layer, lower layer of water continues to add the equal-volume ethyl acetate mutually, extracting twice repeatedly merges the organic phase rotary evaporation of three extractions, adjusts vaporization temperature at 70 ℃, be convenient to the ethyl acetate volatilization, rotary evaporation 0.5 hour concentrates until organic phase, carries out nitrogen again and blows, blow away ethyl acetate, obtain the tea-polyphenol solid; Contain a small amount of tea-polyphenol in the ethyl acetate that rotary evaporation reclaims, can be used for extracting next time; Water reclaims, and wherein contains a small amount of tea-polyphenol, and can be used for next time, tealeaves extracts; Tealeaves hot-water soak caught on a filter is filtered with filter cloth and is pressed dry triplicate; Merge the water that produces in this filtrate and the two kinds of extraction processes, join down batch tealeaves and be used for decocting.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101070665A CN101343270B (en) | 2008-09-04 | 2008-09-04 | Method for extracting tea polyphenol and theine from tea simultaneously |
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| CN2008101070665A CN101343270B (en) | 2008-09-04 | 2008-09-04 | Method for extracting tea polyphenol and theine from tea simultaneously |
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| CN101343270A CN101343270A (en) | 2009-01-14 |
| CN101343270B true CN101343270B (en) | 2011-01-19 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914097B (en) * | 2010-08-02 | 2013-02-13 | 张海 | Technological method for extracting caffeine and tea polyphenol mixture from tea step by step |
| CN102503964B (en) * | 2011-11-11 | 2015-04-22 | 河南大学 | Preparation process for tea polyphenol metal complex |
| CN103242314B (en) * | 2013-04-19 | 2015-06-24 | 天津大学 | Method for comprehensively extracting effective ingredients in tea |
| CN104130260A (en) * | 2014-07-07 | 2014-11-05 | 李华 | Caffeine extraction method |
| CN106690320B (en) * | 2017-01-03 | 2020-10-16 | 武汉轻工大学 | Preparation method of high-purity tea polyphenol |
| CN107759599A (en) * | 2017-10-12 | 2018-03-06 | 贵州省石阡正岩苔生态茶业有限公司 | A kind of method of tealeaves extraction caffeine inferior |
| CN108586458A (en) * | 2018-05-22 | 2018-09-28 | 四川大学 | A method of tealeaves tea polyphenols and caffeine are detached using ionic liquid extract |
| CN111450100A (en) * | 2020-03-30 | 2020-07-28 | 韶关学院 | Camellia nitidissima caffeine and chlorogenic acid composition for resisting novel coronavirus as well as preparation method and application of camellia nitidissima caffeine and chlorogenic acid composition |
| CN114680202B (en) * | 2022-03-04 | 2024-02-09 | 南阳和佳农林科技有限公司 | Tea extracting solution extracting system and method |
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Effective date of registration: 20190522 Address after: 330000 No. 555, Second Axi Lake Road, Nanchang High-tech Development Zone, Jiangxi Province Patentee after: Jiangxi Tongtianle Science & Technology Industrial Co., Ltd. Address before: 330063 No. 696 Fenghe South Avenue, Honggutan New District, Nanchang City, Jiangxi Province Patentee before: Nanchang Univ. of Aviation |
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