CN108892692A - The method that tea polyphenols in fresh tea passes are extracted using resin process - Google Patents
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Abstract
The invention discloses a kind of methods for extracting tea polyphenols in fresh tea passes using resin process, include the following steps：a1：By fresh tea passes after high temperature enzyme deactivation, drying to water content is lower than 6%；a2：Above-mentioned stem tea is crushed, crosses 100 mesh with upper screen cloth；a3：By stem tea powder be placed in 25 DEG C to be lauched in, first impregnate 0.5~1h, then heating extraction, filter and remove residue；a4：3~20g aluminum sulfate, centrifugation first is added by filtered fluid described in every 1L；a5：Ultrafiltration is carried out to tea polyphenols supernatant；a6：Chloroform is added in tea polyphenols ultrafiltrate and stirs, liquid separation again maintains extract liquor between 65~80 DEG C, stirs 1~3min；a7：Tea polyphenols ultrafiltrate is subjected to resin adsorption；a8：It using ethanol solution, is eluted, obtains eluent；a9：Eluent is boiled off into solvent, is dried in vacuo, obtains tea polyphenols finished product.Using this technique, the tea polyphenols purity is high extracted and obtained can be realized, impurity is few, and significantly reduces the maintenance cost of resin column, improves production efficiency.
Description
Technical field
The invention belongs to field of natural product extraction, and in particular to the side of tea polyphenols in fresh tea passes is extracted using resin process
Method.
Background technique
Tea polyphenols (TeaPolyphenols) are the general names of Polyphenols of Tea, including flavanol compound, anthocyanin class,
Flavonoids, flavonols and phenolic acid class etc..Predominantly flavanols (catechin) class, catechin account for 60~80%.Tea polyphenols are also known as
Tea tan or tea tannin, be have in one of main ingredient to form tealeaves color, smell and taste and tealeaves healthcare function main ingredient it
One.Studies have shown that the removing toxic substances of tea polyphenols isoreactivity substance tool and radiation resistance, can effectively stop radioactive substance intrusion bone
Marrow, and strontium 90 and Co 60 can be made to excrete rapidly, " radiation jinx " is described as by health and medical field.
Additive of the tea polyphenols as medicine and food etc., development and application prospect are very good.In addition, with tea polyphenols
Application study is goed deep into, and tea polyphenols also start to be applied in fields such as cosmetics, daily-use chemical industry, light industries.Tea polyphenols mention
Taking technique there has been comparable research at present, and wherein solvent extraction, precipitation by metallic ion are to study and report more extraction method,
There are also some new method reports in recent years, such as resin adsorption method, supercritical fluid extraction, ultrasonic-leaching method, microwave
Extraction etc..But a kind of extracting process is relied solely on, it be easy to cause that extraction efficiency is low, tea polyphenol extract is incomplete or residual
The situation for staying object, impurity more.
The disclosure of background above technology contents is only used for auxiliary and understands inventive concept and technical solution of the invention, not
The prior art for necessarily belonging to present patent application shows above content in the applying date of present patent application in no tangible proof
In the case where having disclosed, above-mentioned background technique should not be taken to the novelty and creativeness of evaluation the application.
Summary of the invention
The technical problem to be solved in the present invention is to provide the methods for extracting tea polyphenols in fresh tea passes using resin process, with reality
The high efficiency extraction of existing tea polyphenols, the tea polyphenols purity is high extracted, impurity is few, and significantly reduces the maintenance cost of resin column,
Improve production efficiency.
In order to solve the above technical problems, the present invention uses following technical scheme：
The method for extracting tea polyphenols in fresh tea passes using resin process, includes the following steps：
a1：It by fresh tea passes after 2~3min of high temperature enzyme deactivation, is dried using cryogenic temperature freezing drying technique, drying is extremely
Water content is lower than 6%；
a2：Above-mentioned stem tea is crushed, 100 mesh is crossed with upper screen cloth, obtains stem tea powder；
a3：By stem tea powder be placed in 25 DEG C to be lauched in, first impregnate 0.5~1h, be then heated to 80~85 DEG C of maintenances
15~30min, filter and remove residue obtain filtered fluid；
a4：3~20g aluminum sulfate first is added by filtered fluid described in every 1L, after concussion, maintain 4~5 DEG C with 3000~
4500rpm is centrifuged 8~12min, obtains tea polyphenols supernatant；
a5：Ultrafiltration membrane of the molecular cut off between 6~80,000 is chosen, ultrafiltration is carried out to tea polyphenols supernatant, obtains tea polyphenols
Ultrafiltrate；
a6：Chloroform is added in tea polyphenols ultrafiltrate and stirs, liquid separation, obtains water layer tea polyphenols extract liquor, recycling examination
Oxidant layer, then water layer tea polyphenols extract liquor is maintained between 65~80 DEG C, 1~3min is stirred, is then down to 40 to fluid temperature
DEG C or less enter resin adsorption link；
a7：Macroporous absorbent resin is flowed through by tea polyphenols ultrafiltrate circulation 2 times to adsorb；
a8：Concentration is used to be washed for 10%~95% ethanol solution by low concentration to eluting in high concentration to resin
De- liquid；
a9：Eluent is placed under 35~40 DEG C of water bath conditions and boils off solvent, is dried in vacuo, obtains tea polyphenols finished product.
Further, the method for extracting tea polyphenols in fresh tea passes using resin process, includes the following steps：
a1：It by fresh tea passes after 2~3min of high temperature enzyme deactivation, is dried using cryogenic temperature freezing drying technique, drying is extremely
Water content is lower than 6%；
a2：Above-mentioned stem tea is crushed, 200 mesh is crossed with upper screen cloth, obtains stem tea powder；
a3：By stem tea powder be placed in 25 DEG C to be lauched in, first impregnate 0.5~1h, be then heated to 80~85 DEG C of maintenances
15~30min, filter and remove residue obtain filtered fluid；
a4：3~20g aluminum sulfate first is added by filtered fluid described in every 1L, after concussion, maintain 4~5 DEG C with 3000~
4500rpm is centrifuged 8~12min, obtains tea polyphenols supernatant；
a5：Ultrafiltration membrane of the molecular cut off between 6~80,000 is chosen, ultrafiltration is carried out to tea polyphenols supernatant, obtains tea polyphenols
Ultrafiltrate；
a6：Chloroform is added in tea polyphenols ultrafiltrate and stirs, liquid separation, obtains water layer tea polyphenols extract liquor, recycling examination
Oxidant layer, then water layer tea polyphenols extract liquor is maintained between 65~70 DEG C, 1~3min is stirred, is then down to 20 to fluid temperature
~25 DEG C or less enter resin adsorption link；
a7：Macroporous absorbent resin is flowed through by tea polyphenols ultrafiltrate circulation 2 times to adsorb；
a8：Concentration is used to be washed for 10%~95% ethanol solution by low concentration to eluting in high concentration to resin
De- liquid；
a9：Eluent is placed under 35~40 DEG C of water bath conditions and boils off solvent, is dried in vacuo, obtains tea polyphenols finished product.
Further, ultrafiltration membrane described in step a5 selects flat plate ultrafiltration membrane, surpasses rate equipment by plate and completes ultra filtration
Journey.
Further, large aperture resin described in step a7 is that the aperture 60~90nm, the AB-8 of 25%~40% cell size are big
Macroporous adsorbent resin.
Further, it is 15~25 DEG C that system temperature is kept in step a7, and flow velocity is 3.5~5.5BV/h.
Further, large aperture resin described in step a7 is the AB-8 macroporous absorbent resin in the aperture 70nm, 30% cell size.
Further, it is 20~25 DEG C that system temperature is kept in step a7, and flow velocity is 4.0~5.0BV/h.
The invention has the advantages that：
Methods of Extraction of Tea-polyphenols of the present invention first passes through cryogenic temperature freezing drying fresh tea passes, removes moisture removal, it is ensured that
It carries out effectivelying prevent the oxidations of tea polyphenols when ultra-fine grinding, by high temperature water leaching, after filter residue, it is heavy big that aluminum sulfate wadding is added
Molecule particles are centrifuged at 3000~4500rpm, centrifugation fall most of bigger molecule impurity, then by ultrafiltration membrane into
One step removes the impurity such as removing protein, polysaccharide, then effectively removes other organic impurities such as caffeine by chloroform, is finally set
Rouge absorption, obtains high-purity tea polypenols, gained finished product tea polyphenols purity is high is up to 90% or more, and each link of this technique is not adopted substantially
Short with high temperature or high-temperature time, therefore, effective tea polyphenols yield is also very high, meanwhile, it is gone based on successively combining to use to be centrifuged
Miscellaneous, ultrafiltration impurity elimination and chloroform organic solution impurity elimination, final to realize when carrying out resin adsorption, impurity is less, significantly mentions
The high service life of resin column, reduces maintenance cost, increases economic efficiency.
Specific embodiment
Invention is further described in detail With reference to embodiment.It is emphasized that following the description is only
It is merely exemplary, the range and its application being not intended to be limiting of the invention.
Embodiment 1：
The method for extracting tea polyphenols in fresh tea passes using resin process, includes the following steps：
a1：It by fresh tea passes after 2~3min of high temperature enzyme deactivation, is dried using cryogenic temperature freezing drying technique, drying is extremely
Water content is lower than 6%；
a2：Above-mentioned stem tea is crushed, net is sieved with 100 mesh sieve, obtains stem tea powder；
a3：By stem tea powder be placed in 25 DEG C to be lauched in, first impregnate 0.5h, be then heated to 85 DEG C of maintenance 15min, mistake
Slag is filtered off, filtered fluid is obtained；
a4：3g aluminum sulfate first is added by filtered fluid described in every 1L, after concussion, maintains 4~5 DEG C and is centrifuged with 3000rpm
12min obtains tea polyphenols supernatant；
a5：Ultrafiltration membrane of the molecular cut off 60,000 or so is chosen, ultrafiltration is carried out to tea polyphenols supernatant, it is super to obtain tea polyphenols
Filtrate, the ultrafiltration membrane select flat plate ultrafiltration membrane, surpass rate equipment by plate and complete ultra-filtration process；
a6：Chloroform is added in tea polyphenols ultrafiltrate and stirs, liquid separation, obtains water layer tea polyphenols extract liquor, recycling examination
Oxidant layer, then water layer tea polyphenols extract liquor is maintained 65 DEG C or so, stirs 2~3min, then to fluid temperature be down to 40 DEG C with
It is lower to enter resin adsorption link；
a7：It is 20~25 DEG C that tea polyphenols ultrafiltrate, which is kept system temperature, and flow velocity is 4.0~4.5BV/h, recycles 2 streams
It is adsorbed through macroporous absorbent resin, the large aperture resin is the AB-8 macroporous absorbent resin in the aperture 60nm, 40% cell size；
a8：Concentration is used to be washed for 10%~95% ethanol solution by low concentration to eluting in high concentration to resin
De- liquid；
a9：Eluent is placed under 35~40 DEG C of water bath conditions and boils off solvent, is dried in vacuo, obtains tea polyphenols finished product.
Embodiment 2
The method for extracting tea polyphenols in fresh tea passes using resin process, includes the following steps：
a1：It by fresh tea passes after 2~3min of high temperature enzyme deactivation, is dried using cryogenic temperature freezing drying technique, drying is extremely
Water content 5% or so；
a2：Above-mentioned stem tea is crushed, 200 mesh screens is crossed, obtains stem tea powder；
a3：By stem tea powder be placed in 25 DEG C to be lauched in, first impregnate 1h, be then heated to 80 DEG C of maintenance 30min, filter
It removes slag, obtains filtered fluid；
a4：10g aluminum sulfate first is added by filtered fluid described in every 1L, after concussion, maintains 4~5 DEG C and is centrifuged with 3500rpm
8min obtains tea polyphenols supernatant；
a5：Ultrafiltration membrane of the molecular cut off 70,000 or so is chosen, ultrafiltration is carried out to tea polyphenols supernatant, it is super to obtain tea polyphenols
Filtrate, the ultrafiltration membrane select flat plate ultrafiltration membrane, surpass rate equipment by plate and complete ultra-filtration process；
a6：Chloroform is added in tea polyphenols ultrafiltrate and stirs, liquid separation, obtains water layer tea polyphenols extract liquor, recycling examination
Oxidant layer, then water layer tea polyphenols extract liquor is maintained 70 DEG C or so, 1~2min is stirred, is then down to 20~25 to fluid temperature
DEG C or less enter resin adsorption link；
a7：It is 20~25 DEG C, flow velocity 5.0BV/h that tea polyphenols ultrafiltrate, which is kept system temperature, recycles 2 times and flows through macropore
Absorption resin is adsorbed, and the large aperture resin is the AB-8 macroporous absorbent resin in the aperture 70nm, 30% cell size；
a8：Concentration is used to be washed for 10%~95% ethanol solution by low concentration to eluting in high concentration to resin
De- liquid；
a9：Eluent is placed under 35~40 DEG C of water bath conditions and boils off solvent, is dried in vacuo, obtains tea polyphenols finished product.
Embodiment 3
a1：It by fresh tea passes after 2~3min of high temperature enzyme deactivation, is dried using cryogenic temperature freezing drying technique, drying is extremely
Water content is lower than 6%；
a2：Above-mentioned stem tea is crushed, 100 mesh is crossed with upper screen cloth, obtains stem tea powder；
a3：By stem tea powder be placed in 25 DEG C to be lauched in, first impregnate 1h, be then heated to 85 DEG C of maintenance 15min, filter
It removes slag, obtains filtered fluid；
a4：20g aluminum sulfate first is added by filtered fluid described in every 1L, after concussion, maintains 4~5 DEG C and is centrifuged with 4500rpm
8min obtains tea polyphenols supernatant；
a5：Ultrafiltration membrane of the molecular cut off 80,000 or so is chosen, ultrafiltration is carried out to tea polyphenols supernatant, it is super to obtain tea polyphenols
Filtrate, the ultrafiltration membrane select flat plate ultrafiltration membrane, surpass rate equipment by plate and complete ultra-filtration process；
a6：Chloroform is added in tea polyphenols ultrafiltrate and stirs, liquid separation, obtains water layer tea polyphenols extract liquor, recycling examination
Oxidant layer, then water layer tea polyphenols extract liquor is maintained 80 DEG C or so, stirs 1min, then to fluid temperature be down to 40 DEG C or less into
Enter resin adsorption link；
a7：It is 20~25 DEG C, flow velocity 5.0BV/h that tea polyphenols ultrafiltrate, which is kept system temperature, recycles 2 times and flows through macropore
Absorption resin is adsorbed, and the large aperture resin is the AB-8 macroporous absorbent resin in the aperture 90nm, 25% cell size；
a8：Concentration is used to be washed for 10%~95% ethanol solution by low concentration to eluting in high concentration to resin
De- liquid；
a9：Eluent is placed under 35~40 DEG C of water bath conditions and boils off solvent, is dried in vacuo, obtains tea polyphenols finished product.
For the beneficial effect that the present invention will be described in detail, it is further provided experimental result.
By equivalent, the same to place of production, with quality fresh tea passes respectively through five kinds of common extracting methods and three embodiment institutes of the invention
It states extracting method and carries out tea polyphenol extract, material used in five kinds of common extracting methods and condition when test are as shown in the table.
The data such as the tea polyphenols purity under the conditions of eight kinds of different purifications, organic solvent residual, impurity residual are detected and record,
As shown in the table.
By experimental result as it can be seen that compared to solvent refluxing extraction, resin extraction, supercritical fluid extraction, column chromatographic extraction
General extraction methods carry out tea polyphenol extract to fresh tea passes using the method for the invention, have the tea polyphenols rate of recovery high, made
Tea polyphenols polyphenol content is high, solvent residual amount is low, Caffeine in Tea Polyphenol content is few advantage.
The specific implementation of the invention is not to be limited to these illustrations for the above content, and technology belonging to the present invention is led
For the those of ordinary skill in domain, without departing from the inventive concept of the premise, a number of simple deductions or replacements can also be made,
It all shall be regarded as belonging to present invention scope of patent protection determined by the appended claims.
Claims (7)
1. the method for extracting tea polyphenols in fresh tea passes using resin process, which is characterized in that include the following steps：
a1：By fresh tea passes after 2~3min of high temperature enzyme deactivation, it is dried using cryogenic temperature freezing drying technique, it is dry to aqueous
Amount is lower than 6%；
a2：Above-mentioned stem tea is crushed, 100 mesh is crossed with upper screen cloth, obtains stem tea powder；
a3：By stem tea powder be placed in 25 DEG C to be lauched in, first impregnate 0.5~1h, be then heated to 80~85 DEG C maintain 15~
30min, filter and remove residue obtain filtered fluid；
a4：3~20g aluminum sulfate first is added by filtered fluid described in every 1L, after concussion, maintain 4~5 DEG C with 3000~4500rpm from
8~12min of the heart obtains tea polyphenols supernatant；
a5：Ultrafiltration membrane of the molecular cut off between 6~80,000 is chosen, ultrafiltration is carried out to tea polyphenols supernatant, obtains tea polyphenols ultrafiltration
Liquid；
a6：It is added and chloroform and stirs, liquid separation in tea polyphenols ultrafiltrate, obtain water layer tea polyphenols extract liquor, reclaim reagent layer,
Water layer tea polyphenols extract liquor is maintained between 65~80 DEG C again, 1~3min is stirred, is then down to 40 DEG C or less to fluid temperature
Into resin adsorption link；
a7：Macroporous absorbent resin is flowed through by tea polyphenols ultrafiltrate circulation 2 times to adsorb；
a8：Concentration is used to be eluted for 10%~95% ethanol solution by low concentration to eluting in high concentration to resin
Liquid；
a9：Eluent is placed under 35~40 DEG C of water bath conditions and boils off solvent, is dried in vacuo, obtains tea polyphenols finished product.
2. the method according to claim 1 for extracting tea polyphenols in fresh tea passes using resin process, which is characterized in that including
Following steps：
a1：By fresh tea passes after 2~3min of high temperature enzyme deactivation, it is dried using cryogenic temperature freezing drying technique, it is dry to aqueous
Amount is lower than 6%；
a2：Above-mentioned stem tea is crushed, 200 mesh is crossed with upper screen cloth, obtains stem tea powder；
a3：By stem tea powder be placed in 25 DEG C to be lauched in, first impregnate 0.5~1h, be then heated to 80~85 DEG C maintain 15~
30min, filter and remove residue obtain filtered fluid；
a4：3~20g aluminum sulfate first is added by filtered fluid described in every 1L, after concussion, maintain 4~5 DEG C with 3000~4500rpm from
8~12min of the heart obtains tea polyphenols supernatant；
a5：Ultrafiltration membrane of the molecular cut off between 6~80,000 is chosen, ultrafiltration is carried out to tea polyphenols supernatant, obtains tea polyphenols ultrafiltration
Liquid；
a6：It is added and chloroform and stirs, liquid separation in tea polyphenols ultrafiltrate, obtain water layer tea polyphenols extract liquor, reclaim reagent layer,
Water layer tea polyphenols extract liquor is maintained between 65~70 DEG C again, 1~3min is stirred, is then down to 20~25 DEG C to fluid temperature
Enter resin adsorption link below；
a7：Macroporous absorbent resin is flowed through by tea polyphenols ultrafiltrate circulation 2 times to adsorb；
a8：Concentration is used to be eluted for 10%~95% ethanol solution by low concentration to eluting in high concentration to resin
Liquid；
a9：Eluent is placed under 35~40 DEG C of water bath conditions and boils off solvent, is dried in vacuo, obtains tea polyphenols finished product.
3. described in any item methods for extracting tea polyphenols in fresh tea passes using resin process according to claim 1~2, feature
It is, ultrafiltration membrane described in step a5 selects flat plate ultrafiltration membrane, surpasses rate equipment by plate and completes ultra-filtration process.
4. described in any item methods for extracting tea polyphenols in fresh tea passes using resin process according to claim 1~2, feature
It is, large aperture resin described in step a7 is the AB-8 macroporous absorbent resin in the aperture 60~90nm, 25%~40% cell size.
5. described in any item methods for extracting tea polyphenols in fresh tea passes using resin process according to claim 1~2, feature
It is, it is 15~25 DEG C that system temperature is kept in step a7, and flow velocity is 3.5~5.5BV/h.
6. the method according to claim 4 for extracting tea polyphenols in fresh tea passes using resin process, which is characterized in that step
Large aperture resin described in a7 is the AB-8 macroporous absorbent resin in the aperture 70nm, 30% cell size.
7. the method according to claim 5 for extracting tea polyphenols in fresh tea passes using resin process, which is characterized in that step
It is 20~25 DEG C that system temperature is kept in a7, and flow velocity is 4.0~5.0BV/h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110590861A (en) * | 2019-09-18 | 2019-12-20 | 紫云自治县新山农业发展有限公司 | Method for extracting tea polyphenol from fresh tea leaves |
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Application publication date: 20181127 |