CN108948101A - The method of ultrasonic supercritical combined extracting tea polyphenols - Google Patents

The method of ultrasonic supercritical combined extracting tea polyphenols Download PDF

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CN108948101A
CN108948101A CN201810669583.5A CN201810669583A CN108948101A CN 108948101 A CN108948101 A CN 108948101A CN 201810669583 A CN201810669583 A CN 201810669583A CN 108948101 A CN108948101 A CN 108948101A
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tea polyphenols
neopelex
extraction
supercritical
fluid
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吴思祥
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Guangxi Clooney Tea Biotechnology Co Ltd
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Guangxi Clooney Tea Biotechnology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
    • C07G99/00—Subject matter not provided for in other groups of this subclass
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00—Tea; Tea substitutes; Preparations thereof
    • A23F3/16—Tea extraction; Tea extracts; Treating tea extract; Making instant tea
    • A23F3/18—Extraction of water soluble tea constituents
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention discloses a kind of methods of ultrasonic supercritical combined extracting tea polyphenols, belong to tea polyphenol extract technical field.The method of the ultrasonic supercritical combined extracting tea polyphenols includes feedstock processing, ultrasonication, supercritical CO2It extracts, isolate and purify.Tea polyphenols are extracted using above method, the recovery rate and purity of tea polyphenols can be improved.

Description

The method of ultrasonic supercritical combined extracting tea polyphenols
Technical field
The invention belongs to tea polyphenol extract technical fields, and in particular to the side of ultrasonic supercritical combined extracting tea polyphenols Method.
Background technique
Tea polyphenols (Tea Polyphenols) are the general name 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.
Tea polyphenols are extracted from tealeaves, have effects that more comprehensive, and the content of Tea Polyphenols in Tea is percentage 20-30%.Tea polyphenols have very strong antioxidation, have inhibiting effect to clostridiopetidase A and elastoser, can prevent elasticity The content of albumen declines or denaturation, maintains skin elasticity, reaches wrinkle-proof effect.Tea polyphenols can absorb ultraviolet light, reduce melanin Growth, have inhibiting effect to tyrosinase and peroxidase, to reach whitening function.Polyphenol is one kind in ultraviolet area There are the natural products of strong absorbent, and property nontoxic to the human body.By the compounding of several polyphenol and flavones, its ultraviolet region is utilized The sun-proof composite natural ultraviolet absorbent of wide spectrum can be obtained in the difference of absorption, plays the formation for reducing dermal melanin, prevents skin old The effect of change.
Traditional tea polyphenol extract uses solvent extraction, and tea polyphenol extract rate is low (general recovery rate is 5%-6%), product Purity is low, and product is oxidizable, and wherein contains a large amount of impurities (such as plant polyose, tea brown pigment, pigment, caffeine, resin). It is extracted with organic solvent, though recovery rate can increase and (can reach 1O%-15%), due to not only more containing tea in leaching liquor Phenol, but also containing the impurity such as Tea Pigment, caffeine, will obtain fine work, must also impurity removal and purification repeatedly, process is more, and technique is cumbersome Complexity, extraction process generally need to be through 3 grades of cross current solvent extractions；It need to repeatedly distill, heating time is long；It needs with a large amount of organic solvent, Some organic solvent recycling are difficult, toxic, inflammable, are unfavorable for keeping the safety in production.
Chinese patent literature " ultrasonic supercritical combined extracting Tea Polyphenols (patent No.: ZL201310683801.8) " Disclose a kind of method extraction tea polyphenols combined using ultrasonic wave and supercritical extract, including smashing, microwave treatment, ultrasonic wave Processing, again with by spraying settle high-purity tea polypenols are made.The invention has the characteristics that shorten the tea polyphenol extract time, but exists and mention Take rate not high, the problems such as tea polyphenols purity is not high.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of ultrasonic supercritical combined extracting tea polyphenols, to solve tea polyphenols Recovery rate and the low problem of purity.
In order to solve the above technical problems, the invention adopts the following technical scheme:
The method of ultrasonic supercritical combined extracting tea polyphenols, including feedstock processing, ultrasonication, supercritical CO2Extraction divides From purification step, wherein supercritical CO2Extraction the following steps are included:
The slurries of processing are used into supercritical CO2Extraction, in CO2Neopelex is added in fluid, ethyl acetate, gathers Sorb ester controls extracting pressure and temperature, CO2Flow is 20-25L/h, and extraction time 1.5-3.5h obtains tea polyphenols crude product A separates tea polyphenols crude product with slurries, separating pressure 3-6Mpa, and separation temperature is 40-50 DEG C；Remaining slurries use again Supercritical CO2Extraction, in CO2Acetone, neopelex are added in fluid, controls extracting pressure and temperature, CO2Flow For 20-25L/h, extraction time 1-2h, tea polyphenols crude product b is obtained, tea polyphenols crude product is separated with slurries, separating pressure 3- 6Mpa, separation temperature are 40-50 DEG C, and gained tea polyphenols crude product a and tea polyphenols crude product b are mixed, hydrochloric acid is added, and adjust pH value and are 3-5.2 is centrifuged or is separated by filtration, obtains millet paste.
Further, the neopelex, ethyl acetate, polysorbate total dosage be CO2Fluid 18%-25%, wherein neopelex, ethyl acetate, polysorbate weight proportion be (1.5-2.8): (0.6-2): (1.5-3).
Further, the neopelex, ethyl acetate, polysorbate weight proportion be 2.3:2:2.6.
Further, in CO2Neopelex, ethyl acetate, polysorbate, control extraction pressure are added in fluid Power is 26-30MPa.
Further, in CO2Neopelex, ethyl acetate, polysorbate, control extraction temperature are added in fluid Degree is 52-58 DEG C.
Further, the acetone, neopelex total dosage be CO2The 14%-20% of fluid, wherein third Ketone, neopelex weight proportion be (1-2): (0.5-1.2).
Further, the acetone, neopelex weight proportion be 1.6:1.
Further, in CO2Acetone, neopelex are added in fluid, control extracting pressure is 22-27MPa.
Further, in CO2Acetone, neopelex are added in fluid, control extraction extraction temperature is 50-56 ℃。
Further, the concentration of the hydrochloric acid is 18%-28%, and dosage is the 6%-16% of tea polyphenols crude product total amount.
The invention has the following advantages:
(1) by the data of embodiment 1-3 and comparative example 5 as it can be seen that the recovery rate of tea polyphenols and purity are significantly higher than in embodiment 1-3 The recovery rate and purity of tea polyphenols in comparative example 5；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is optimum embodiment.
(2) by embodiment 2 and the data of comparative example 1-4 as it can be seen that step S1 adds ethyl alcohol in water pasty slurry, with The operating procedure of the speed stirring 15min of 400r/min；Lack in step S3 in CO2CO is added in fluid2Fluid volume 22% The operating procedure of neopelex, ethyl acetate, polysorbate；Lack addition hydrochloric acid in step S3, adjusting pH value is 4.8 operating procedure, plays synergistic effect during extracting tea polyphenols, and collaboration improves the recovery rate of tea polyphenols and pure Degree；This is:
Ethyl alcohol is added in step S1 in water pasty slurry, the ethyl alcohol of addition is polar solvent, and tea polyphenols are also polar substances, root According to the principle of similar compatibility, ethyl alcohol can promote the dissolution of tea polyphenols in water, the dissolution without influencing other apolar substances Rate；Heating water bath and 15min is stirred simultaneously with the speed of 400r/min, so that green tea internal temperature increases, stirring can accelerate The diffusion of the extracts such as tea polyphenols, and then it is leached out tea polyphenols quickly, to increase the recovery rate and purity of tea polyphenols.By In tea polyphenols in CO2Solubility in fluid is little, causes its recovery rate not high, the present invention has according to neopelex There is surfactant property, solution can be made sufficiently to activate, the characteristics of tea polyphenols are soluble in ethyl acetate and polysorbate are as increasing Solvent can form micelle in water, Adsorption of Tea Polyphenols substance and increase tea polyphenols in CO2The features such as solubility in fluid, in step To CO in rapid S32CO is added in fluid2Neopelex, ethyl acetate, the polysorbate of fluid volume 22%, it is possible to increase Tea polyphenols are in CO2Solubility in fluid；On the basis of adding ethyl alcohol into water pasty slurry in step sl, in conjunction with dodecane Base benzene sulfonic acid sodium salt has surfactant property, solution can be made sufficiently to activate and the characteristics of tea polyphenols are soluble in ethyl acetate, into The recovery rate of one step increase tea polyphenols.Tea polyphenols are stable in acid condition, oxidizable under alkaline condition, and step S3 is more in tea Acetic acid is added after phenol extraction separation, adjusting pH value is 4.8, tea polyphenols can be prevented to be oxidized, to improve the purity of tea polyphenols.
Specific embodiment
In order to better understand the present invention, it is first illustrated using following implementation, following embodiment belongs to the present invention Protection scope, but do not limit the scope of the invention.
The method of the ultrasonic supercritical combined extracting tea polyphenols, comprising the following steps:
S1: green tea is dried and is ground into 50-100 mesh, then adds distilled water, is placed in vacuum high shear homogenizer sufficiently even Matter obtains water pasty slurry, then uses heating water bath, makes the control of water pasty slurry temperature at 53-72 DEG C, and starches in water paste Ethyl alcohol is added in material, 15-20min is stirred with the speed of 300-400r/min, obtains slurries, the green tea after placing cooling 0.5-1h The amount ratio of leaf and distilled water is 1:8-17, and the concentration of the ethyl alcohol is 25%-30%, and the amount ratio of green tea and ethyl alcohol is 1: 0.4-0.6；
S2: carrying out ultrasonication to slurries, and the frequency of the ultrasonic wave is 25-30KHz, and the processing time is 5-8min, is made The slurries of processing；
S3: the slurries handled through step S2 are used into supercritical CO2Extraction, in CO2In fluid be added neopelex, Ethyl acetate, polysorbate, the neopelex, ethyl acetate, polysorbate total dosage be CO2Fluid 18%-25%, wherein neopelex, ethyl acetate, polysorbate weight proportion be (1.5-2.8): (0.6-2): (1.5-3), control extracting pressure are 26-30MPa, and extraction temperature is 52-58 DEG C, CO2Flow is 20-25L/h, and extraction time is 1.5-3.5h obtains tea polyphenols crude product a, tea polyphenols crude product is separated with slurries, separating pressure 3-6Mpa, and separation temperature is 40-50℃；Remaining slurries use supercritical CO again2Extraction, in CO2Acetone, neopelex, institute are added in fluid State acetone, total dosage of neopelex is CO2The 14%-20% of fluid, wherein acetone, neopelex Weight proportion is (1-2): (0.5-1.2), and control extracting pressure is 22-27MPa, and extraction temperature is 50-56 DEG C, CO2Flow is 20-25L/h, extraction time 1-2h obtain tea polyphenols crude product b, tea polyphenols crude product are separated with slurries, separating pressure 3- 6Mpa, separation temperature are 40-50 DEG C, and gained tea polyphenols crude product a and tea polyphenols crude product b are mixed, hydrochloric acid is added, the hydrochloric acid Concentration is 18%-28%, and dosage is the 6%-16% of tea polyphenols crude product total amount, and adjusting pH value is 3-5.2, is centrifuged or is separated by filtration, obtains To millet paste；
S4: by LX-8 type large pore resin absorption column on millet paste, the diameter height of LX-8 type large pore resin absorption column compares for 1:5-15, loading Amount is 37-56 times of column volume, and loading flow velocity is 0 .5-2 BV/h, the ethanol water for being first 1.2-7.5% with volume fraction Elution removal of impurities, dosage is 20-26 times of column volume, flow velocity is 1-4 BV/h, then the ethanol water for being 56%-73% with volume fraction Solution elution, dosage is 12-18 times of column volume, flow velocity is 1-4 BV/h, and collected volume score is the ethanol water of 56%-73% The eluent of solution is concentrated under reduced pressure, and tea polyphenols product is made in spray drying or freeze-drying.
Embodiment 1
A kind of method of ultrasonic supercritical combined extracting tea polyphenols, comprising the following steps:
S1: green tea is dried and is ground into 80 mesh, then adds distilled water, be placed in vacuum high shear homogenizer sufficiently it is homogeneous, Water pasty slurry is obtained, heating water bath is then used, adds the control of water pasty slurry temperature at 65 DEG C, and in water pasty slurry Add ethyl alcohol, 15min is stirred with the speed of 400r/min, obtains slurries, the use of the green tea and distilled water after placing cooling 0.8h Amount is than being 1:12, and the concentration of the ethyl alcohol is 28%, and the amount ratio of green tea and ethyl alcohol is 1:0.5；
S2: carrying out ultrasonication to slurries, and the frequency of the ultrasonic wave is 30KHz, and the processing time is 5min, and processing is made Slurries；
S3: the slurries handled through step S2 are used into supercritical CO2Extraction, in CO2In fluid be added neopelex, Ethyl acetate, polysorbate, the neopelex, ethyl acetate, polysorbate total dosage be CO2Fluid 22%, wherein neopelex, ethyl acetate, polysorbate weight proportion be 2.3:2:2.6, control extracting pressure For 28MPa, extraction temperature is 56 DEG C, CO2Flow is 23L/h, extraction time 2.5h, tea polyphenols crude product a is obtained, by tea polyphenols Crude product is separated with slurries, separating pressure 5Mpa, and separation temperature is 45 DEG C；Remaining slurries use supercritical CO again2Extraction, CO2In fluid be added acetone, neopelex, the acetone, neopelex total dosage be CO2Fluid 18%, wherein acetone, neopelex weight proportion be 1.6:1, control extracting pressure be 25MPa, extraction temperature It is 55 DEG C, CO2Flow is 22L/h, extraction time 1.5h, obtains tea polyphenols crude product b, and tea polyphenols crude product is separated with slurries, Separating pressure is 5Mpa, and separation temperature is 46 DEG C, and gained tea polyphenols crude product a and tea polyphenols crude product b are mixed, hydrochloric acid, institute are added The concentration for stating hydrochloric acid is 25%, and dosage is the 20% of tea polyphenols crude product total amount, and adjusting pH value is 4.8, is centrifuged or is separated by filtration, obtains Millet paste；
S4: by LX-8 type large pore resin absorption column on millet paste, the diameter height of LX-8 type large pore resin absorption column compares for 1:10, applied sample amount It is 50 times of column volume, loading flow velocity is 1.5 BV/h, and the ethanol aqueous wash removing for being first 5.2% with volume fraction is miscellaneous, is used Amount is 23 times of column volume, flow velocity is 3 BV/h, then the ethanol water for being 65% with volume fraction elutes, and dosage is cylinder Long-pending 15 times, flow velocity be 3 BV/h, the eluent for the ethanol water that collected volume score is 65% is concentrated under reduced pressure, spray drying Or freeze-drying, tea polyphenols product is made.
Embodiment 2
A kind of method of ultrasonic supercritical combined extracting tea polyphenols, comprising the following steps:
S1: green tea is dried and is ground into 50 mesh, then adds distilled water, be placed in vacuum high shear homogenizer sufficiently it is homogeneous, Water pasty slurry is obtained, heating water bath is then used, adds the control of water pasty slurry temperature at 55 DEG C, and in water pasty slurry Add ethyl alcohol, 20min is stirred with the speed of 300r/min, obtains slurries, the use of the green tea and distilled water after placing cooling 0.5h Amount is than being 1:8, and the concentration of the ethyl alcohol is 25%, and the amount ratio of green tea and ethyl alcohol is 1:0.4；
S2: carrying out ultrasonication to slurries, and the frequency of the ultrasonic wave is 25KHz, and the processing time is 8min, and processing is made Slurries；
S3: the slurries handled through step S2 are used into supercritical CO2Extraction, in CO2In fluid be added neopelex, Ethyl acetate, polysorbate, the neopelex, ethyl acetate, polysorbate total dosage be CO2Fluid 19%, wherein neopelex, ethyl acetate, polysorbate weight proportion be 1.5:0.7:1.8, control extraction pressure Power is 26MPa, and extraction temperature is 52 DEG C, CO2Flow is 25L/h, extraction time 3.5h, obtains tea polyphenols crude product a, and tea is more Phenol crude product is separated with slurries, separating pressure 3Mpa, and separation temperature is 40 DEG C；Remaining slurries use supercritical CO again2Extraction, In CO2In fluid be added acetone, neopelex, the acetone, neopelex total dosage be CO2Stream The 14% of body, wherein acetone, neopelex weight proportion be 1:0.5, extraction temperature be 52 DEG C, CO2Flow is 22L/h, extraction time 1.3h obtain tea polyphenols crude product b, tea polyphenols crude product are separated with slurries, separating pressure 5Mpa, point It is 43 DEG C from temperature, gained tea polyphenols crude product a and tea polyphenols crude product b is mixed, add hydrochloric acid, the concentration of the hydrochloric acid is 22%, Dosage is the 13% of tea polyphenols crude product total amount, and adjusting pH value is 3.3, is centrifuged or is separated by filtration, obtains millet paste；
S4: by LX-8 type large pore resin absorption column on millet paste, the diameter height of LX-8 type large pore resin absorption column compares for 1:6, applied sample amount It is 40 times of column volume, loading flow velocity is 0.8BV/h, and the ethanol aqueous wash removing for being first 1.5% with volume fraction is miscellaneous, is used Amount is 22 times, flow velocity 2BV/h of column volume, then the ethanol water for being 60% with volume fraction elutes, and dosage is column volume 13 times, flow velocity be 2 BV/h, collected volume score be 60% ethanol water eluent, be concentrated under reduced pressure, spray drying or Tea polyphenols product is made in freeze-drying.
Embodiment 3
A kind of method of ultrasonic supercritical combined extracting tea polyphenols, comprising the following steps:
S1: green tea is dried and is ground into 100 mesh, then adds distilled water, be placed in vacuum high shear homogenizer sufficiently it is homogeneous, Water pasty slurry is obtained, heating water bath is then used, adds the control of water pasty slurry temperature at 70 DEG C, and in water pasty slurry Add ethyl alcohol, 15min is stirred with the speed of 400r/min, obtains slurries, the dosage of the green tea and distilled water after placing cooling 1h Than being 30% for the concentration of 1:17, the ethyl alcohol, the amount ratio of green tea and ethyl alcohol is 1:0.5；
S2: carrying out ultrasonication to slurries, and the frequency of the ultrasonic wave is 30KHz, and the processing time is 5min, and processing is made Slurries；
S3: the slurries handled through step S2 are used into supercritical CO2Extraction, in CO2In fluid be added neopelex, Ethyl acetate, polysorbate, the neopelex, ethyl acetate, polysorbate total dosage be CO2Fluid 25%, wherein neopelex, ethyl acetate, polysorbate weight proportion be 2.6:2:3, control extracting pressure be 30MPa, extraction temperature are 52 DEG C, CO2Flow is 21L/h, extraction time 2h, obtains tea polyphenols crude product a, by tea polyphenols crude product It is separated with slurries, separating pressure 3.5Mpa, separation temperature is 42 DEG C；Remaining slurries use supercritical CO again2Extraction, in CO2 In fluid be added acetone, neopelex, the acetone, neopelex total dosage be CO2Fluid 20%, wherein acetone, neopelex weight proportion be 2:1.2, control extracting pressure is 22MPa, and extraction temperature is 52 DEG C, CO2Flow is 25L/h, extraction time 1h, obtains tea polyphenols crude product b, and tea polyphenols crude product is separated with slurries, separation Pressure is 3Mpa, and separation temperature is 40 DEG C, and gained tea polyphenols crude product a and tea polyphenols crude product b are mixed, hydrochloric acid, the salt are added The concentration of acid is 28%, and dosage is the 6% of tea polyphenols crude product total amount, and adjusting pH value is 5.2, is centrifuged or is separated by filtration, obtains millet paste；
S4: by LX-8 type large pore resin absorption column on millet paste, the diameter height of LX-8 type large pore resin absorption column compares for 1:15, applied sample amount It is 56 times of column volume, loading flow velocity is 2 BV/h, first removes miscellaneous, dosage with the ethanol aqueous wash that volume fraction is 7.5% For 26 times of column volume, flow velocity be 4 BV/h, then the ethanol water for being 73% with volume fraction elutes, and dosage is column volume 18 times, flow velocity be 4 BV/h, collected volume score be 70% ethanol water eluent, be concentrated under reduced pressure, spray drying or Tea polyphenols product is made in freeze-drying.
Comparative example 1
Preparation method is substantially the same manner as Example 1, has only the difference is that lacking in step S1 and adds ethyl alcohol in water pasty slurry, With the operating procedure of the speed stirring 15min of 400r/min；Lack in step S3 in CO2CO is added in fluid2Fluid volume 22% Neopelex, ethyl acetate, polysorbate operating procedure；Lack addition hydrochloric acid in step S3, adjusts pH value For 4.8 operating procedure.
Comparative example 2
Preparation method is substantially the same manner as Example 1, has only the difference is that lacking in step S1 and adds ethyl alcohol in water pasty slurry, With the operating procedure of the speed stirring 15min of 400r/min.
Comparative example 3
Preparation method is substantially the same manner as Example 1, has only the difference is that lacking in step s3 in CO2CO is added in fluid2Stream The operating procedure of the neopelex of body dosage 22%, ethyl acetate, polysorbate.
Comparative example 4
Preparation method is substantially the same manner as Example 1, has only the difference is that lacking addition hydrochloric acid in step s3, adjusting pH value is 4.8 operating procedure.
Comparative example 5
Using Chinese patent literature " ultrasonic supercritical combined extracting Tea Polyphenols (patent No.: ZL201310683801.8) " The method of middle embodiment 1-3 extracts tea polyphenols.
The tea polyphenols in green tea are extracted according to embodiment 1-3 and comparative example 1-5 the method, every group of experimental example takes 5kg Green tea detects tea polyphenol extract rate and purity, as a result as shown in the table below:
Experimental project Recovery rate (%) Purity (%)
Embodiment 1 18.25 99.91
Embodiment 2 17.89 99.79
Embodiment 3 18.03 99.85
Comparative example 1 11.65 97.21
Comparative example 2 16.46 99.34
Comparative example 3 16.08 99.06
Comparative example 4 16.32 99.18
Comparative example 5 11.79-11.82 98.18-98.26
As seen from the above table: (1) by the data of embodiment 1-3 and comparative example 5 as it can be seen that in embodiment 1-3 the recovery rate of tea polyphenols and Purity is significantly higher than the recovery rate and purity of tea polyphenols in comparative example 5；Simultaneously by the data of embodiment 1-3 as it can be seen that embodiment 1 is Optimum embodiment.
(2) by embodiment 2 and the data of comparative example 1-4 as it can be seen that step S1 adds ethyl alcohol in water pasty slurry, with The operating procedure of the speed stirring 15min of 400r/min；Lack in step S3 in CO2CO is added in fluid2Fluid volume 22% The operating procedure of neopelex, ethyl acetate, polysorbate；Lack addition hydrochloric acid in step S3, adjusting pH value is 4.8 operating procedure, plays synergistic effect during extracting tea polyphenols, and collaboration improves the recovery rate of tea polyphenols and pure Degree；This is:
Ethyl alcohol is added in step S1 in water pasty slurry, the ethyl alcohol of addition is polar solvent, and tea polyphenols are also polar substances, root According to the principle of similar compatibility, ethyl alcohol can promote the dissolution of tea polyphenols in water, the dissolution without influencing other apolar substances Rate；Heating water bath and 15min is stirred simultaneously with the speed of 400r/min, so that green tea internal temperature increases, stirring can accelerate The diffusion of the extracts such as tea polyphenols, and then it is leached out tea polyphenols quickly, to increase the recovery rate and purity of tea polyphenols.By In tea polyphenols in CO2Solubility in fluid is little, causes its recovery rate not high, the present invention has according to neopelex There is surfactant property, solution can be made sufficiently to activate, the characteristics of tea polyphenols are soluble in ethyl acetate and polysorbate are as increasing Solvent can form micelle in water, Adsorption of Tea Polyphenols substance and increase tea polyphenols in CO2The features such as solubility in fluid, in step To CO in rapid S32CO is added in fluid2Neopelex, ethyl acetate, the polysorbate of fluid volume 22%, it is possible to increase Tea polyphenols are in CO2Solubility in fluid；On the basis of adding ethyl alcohol into water pasty slurry in step sl, in conjunction with dodecane Base benzene sulfonic acid sodium salt has surfactant property, solution can be made sufficiently to activate and the characteristics of tea polyphenols are soluble in ethyl acetate, into The recovery rate of one step increase tea polyphenols.Tea polyphenols are stable in acid condition, oxidizable under alkaline condition, and step S3 is more in tea Acetic acid is added after phenol extraction separation, adjusting pH value is 4.8, tea polyphenols can be prevented to be oxidized, to improve the purity of tea polyphenols.
The above content is it cannot be assumed that present invention specific implementation is only limited to these instructions, for the technical field of the invention Those of ordinary skill for, under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all answers When being considered as belonging to present invention scope of patent protection determined by the appended claims.

Claims (10)

1. the method for ultrasonic supercritical combined extracting tea polyphenols, including feedstock processing, ultrasonication, supercritical CO2Extraction, Purification procedures, which is characterized in that supercritical CO2Extraction the following steps are included:
The slurries of processing are used into supercritical CO2Extraction, in CO2Neopelex is added in fluid, ethyl acetate, gathers Sorb ester controls extracting pressure and temperature, CO2Flow is 20-25L/h, and extraction time 1.5-3.5h obtains tea polyphenols crude product A separates tea polyphenols crude product with slurries, separating pressure 3-6Mpa, and separation temperature is 40-50 DEG C；Remaining slurries use again Supercritical CO2Extraction, in CO2Acetone, neopelex are added in fluid, controls extracting pressure and temperature, CO2Flow For 20-25L/h, extraction time 1-2h, tea polyphenols crude product b is obtained, tea polyphenols crude product is separated with slurries, separating pressure 3- 6Mpa, separation temperature are 40-50 DEG C, and gained tea polyphenols crude product a and tea polyphenols crude product b are mixed, hydrochloric acid is added, and adjust pH value and are 3-5.2 is centrifuged or is separated by filtration, obtains millet paste.
2. the method for ultrasonic supercritical combined extracting tea polyphenols according to claim 1, which is characterized in that described 12 Sodium alkyl benzene sulfonate, ethyl acetate, polysorbate total dosage be CO2The 18%-25% of fluid, wherein dodecyl benzene sulfonic acid Sodium, ethyl acetate, polysorbate weight proportion be (1.5-2.8): (0.6-2): (1.5-3).
3. the method for ultrasonic supercritical combined extracting tea polyphenols according to claim 2, which is characterized in that described 12 Sodium alkyl benzene sulfonate, ethyl acetate, polysorbate weight proportion be 2.3:2:2.6.
4. the method for ultrasonic supercritical combined extracting tea polyphenols according to claim 1, which is characterized in that in CO2Fluid Middle addition neopelex, ethyl acetate, polysorbate, control extracting pressure are 26-30MPa.
5. the method for ultrasonic supercritical combined extracting tea polyphenols according to claim 1, which is characterized in that in CO2Fluid Middle addition neopelex, ethyl acetate, polysorbate, control extraction temperature are 52-58 DEG C.
6. the method for ultrasonic supercritical combined extracting tea polyphenols according to claim 1, which is characterized in that described third Ketone, neopelex total dosage be CO2The 14%-20% of fluid, the wherein weight of acetone, neopelex Proportion is (1-2): (0.5-1.2).
7. the method for ultrasonic supercritical combined extracting tea polyphenols according to claim 6, which is characterized in that described third Ketone, neopelex weight proportion be 1.6:1.
8. the method for ultrasonic supercritical combined extracting tea polyphenols according to claim 1, which is characterized in that in CO2Fluid Middle addition acetone, neopelex, control extracting pressure are 22-27MPa.
9. the method for ultrasonic supercritical combined extracting tea polyphenols according to claim 1, which is characterized in that in CO2Fluid Middle addition acetone, neopelex, control extraction extraction temperature is 50-56 DEG C.
10. the method for ultrasonic supercritical combined extracting tea polyphenols according to claim 1, which is characterized in that the salt The concentration of acid is 18%-28%, and dosage is the 6%-16% of tea polyphenols crude product total amount.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112961136A (en) * 2021-02-06 2021-06-15 云南省烟草公司玉溪市公司 Method for extracting polyphenol from tobacco leaves

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103704421A (en) * 2013-12-13 2014-04-09 福州市东苹企业管理服务有限公司 Ultrasonic supercritical combined extraction technology for tea polyphenol
CN104186808A (en) * 2014-09-10 2014-12-10 江苏吟春碧芽股份有限公司 Tea leaf ingredient extracting process

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103704421A (en) * 2013-12-13 2014-04-09 福州市东苹企业管理服务有限公司 Ultrasonic supercritical combined extraction technology for tea polyphenol
CN104186808A (en) * 2014-09-10 2014-12-10 江苏吟春碧芽股份有限公司 Tea leaf ingredient extracting process

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
胥佰涛,ET AL.,: "茶多酚提取方法研究进展", 《茶叶》 *
雷志伟,等，: "茶叶中茶多酚提取技术进展", 《茶叶中茶多酚提取技术进展》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112961136A (en) * 2021-02-06 2021-06-15 云南省烟草公司玉溪市公司 Method for extracting polyphenol from tobacco leaves

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