CN102516245A - Method for extracting caffeine from green tea - Google Patents
Method for extracting caffeine from green tea Download PDFInfo
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- CN102516245A CN102516245A CN2011104032099A CN201110403209A CN102516245A CN 102516245 A CN102516245 A CN 102516245A CN 2011104032099 A CN2011104032099 A CN 2011104032099A CN 201110403209 A CN201110403209 A CN 201110403209A CN 102516245 A CN102516245 A CN 102516245A
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- trimethyl
- xanthine
- green tea
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Abstract
The invention discloses a method for extracting caffeine from green tea. According to the invention, green tea is added to a sulfuric acid extracting solution containing sodium salt or sylvite; homogenization is carried out; a pH value is regulated; an obtained solution is subject to operations such as ultrasonic wave treatment and centrifugal sedimentation, such that solid-liquid separation is carried out; the pH value of an extraction liquid is regulated to basic; the extraction liquid is subject to organic solvent extraction; an extraction liquid is subject to concentration and chromatography, such that a caffeine finished product is obtained. The method provided by the invention is advantaged in simple technology, short production period, high extraction efficiency, and low pollution. The method can easily be applied in productions.
Description
Technical field
The present invention relates to natural medicine field, particularly a kind of method that adopts ultrasonic wave extraction from green tea, to extract trimethyl-xanthine.
Background technology
There is the history of drinking tea of two thousand years in China, and people recognize for a long time to drink tea and can keep fit to get rid of illness.In recent years research shows: the diuresis of not only can refreshing oneself of drinking tea also has inhibiting bacteria and diminishing inflammation, reduce fat, blood sugar and blood pressure, anti-ageing, radioprotective, anti-cancer, biological characteristics such as anticancer.Staple in the tealeaves is a trimethyl-xanthine; Belong to stimulant; Content is about 2%～5% in giving birth to tea, in the finite concentration scope, human body is had physiological action and health-care effects such as cardiac stimulant, diuresis, detoxifcation; Be the important source of medical theine, the process for extracting of trimethyl-xanthine mainly contains four types of solvent method, subliming method, absorption method and supercritical co gas formulations (being called for short the SFE method).Solvent method exists that product purity is low, poor stability (toxic reagent commonly used is made extraction agent), shortcomings such as complex process; Absorption method exists more than the eluent consumption or the use of poisonous eluent; SFE method production cost is higher, still is in the laboratory study stage; The easy carbonization of the direct subliming method of traditional green tea, trimethyl-xanthine purity is low, shortcoming such as loss is bigger during collection.
Summary of the invention
The objective of the invention is to provide that a kind of technical process is simple, extraction yield is high, the method for from green tea, extracting trimethyl-xanthine of environmentally safe to the deficiency of prior art.
In order to achieve the above object; The technical scheme that the present invention adopts is: green tea is added to extract in the solution process homogenate; Solid-liquid separation is carried out in homogenate after ultrasonication, extracting solution is through overregulating pH value, organic solvent extraction, and extraction liquid is again through concentrating, obtaining the trimethyl-xanthine finished product behind the purifying.
Advantage of the present invention: technical process is simple, is easy to promote environmentally safe; Adopt ultrasonic extraction, have advantage with short production cycle, that extraction yield is high.
Embodiment
Below in conjunction with specific embodiment the present invention is done further explain.
The method of from green tea, extracting trimethyl-xanthine provided by the present invention, concrete steps are following:
(1) with green tea, extract solution and add simultaneously and carry out homogenate in the refiner, with 0.5～5% aqueous sulfuric acid the pH value of homogenate is transferred to 2～3.5 then.Said extraction solution is the mixing solutions of aqueous sulfuric acid and inorganic salt solution, and wherein the pH of mixing solutions is 2～3.5, and the volumetric molar concentration of inorganic salt is 1.0M～3.0M.Said inorganic salt are a kind of or mixing more than two kinds wherein of sodium-chlor, Repone K, sodium sulfate or vitriolate of tartar.
(2) use the ultrasonic extraction machine with the ultrasonication homogenate of frequency as 20KHz～1MHz, to increase the stripping quantity of trimethyl-xanthine, the time is 10～90 minutes.
(3) adopt the centrifugal solid matter of removing of settling centrifuge to obtain extracting solution, rotating speed is 1000～6000 rpms, 3～20 minutes time.
(4) with strong aqua the pH value of extracting solution is transferred to 8～11, extract with organic solvent then.Said organic solvent is an ETHYLE ACETATE.
(5) extraction liquid is concentrated into the dried trimethyl-xanthine mixture that obtains under 35～50 ℃ of temperature, negative pressure 0.07～0.1MPa or normal pressure.
(6) with normal phase silicagel column the trimethyl-xanthine mixture is carried out purifying, used elutriant is the chloroform soln that contains 3～10% methyl alcohol.Carry out wash-out with elutriant, merge the elutriant that contains trimethyl-xanthine then, obtain the trimethyl-xanthine bullion at 35～50 ℃ of temperature, negative pressure 0.06～0.1MPa condition recover solvent.
(7) gained trimethyl-xanthine bullion is carried out recrystallization and promptly get the trimethyl-xanthine product; Used recrystallization solvent is 85%～95% ethanolic soln.
Embodiment one
The green tea 100kg of water ratio 42% and extracting solution (the pH value is 2.5 aqueous sulfuric acid, contains 1M sodium-chlor) 100L mixed drop into refiner simultaneously and carry out homogenate, homogenate transfers to pH2.5 with 2% aqueous sulfuric acid; Homogenate is squeezed into the ultrasonic extraction machine through rotor pump; 50KHz ultrasonication 30 minutes, homogenate are centrifugal in rotor pump is squeezed into settling centrifuge again, and rotating speed is 3000 rpms; 20 minutes time, collect supernatant.Throw out is added new extracting solution repeat aforesaid operations 3 times, merge supernatant, with strong aqua adjust pH to 8～9; Place extractor with the ETHYLE ACETATE of 1/2 volume, stir extraction 10 minutes, left standstill 10 minutes; Is that 30 ℃, negative pressure are that the solvent thickener of 0.1MPa reclaims ETHYLE ACETATE with acetic acid ethyl acetate extract through temperature; Extraction liquid is concentrated into dried, after crystallization and purification on normal-phase silica gel column chromatography for separation, obtains the trimethyl-xanthine 2.65g of purity 95.2 again through recrystallization.
Embodiment two
The green tea 100kg of water ratio 20% and extracting solution (the pH value is 3 aqueous sulfuric acid, contains 2M sodium sulfate) 100L mixed drop into refiner simultaneously and carry out homogenate, homogenate transfers to pH3.5 with 2% aqueous sulfuric acid; Homogenate is squeezed into the ultrasonic extraction machine through rotor pump; 1MHz ultrasonication 30 minutes, homogenate are centrifugal in rotor pump is squeezed into settling centrifuge again, and rotating speed is 5000 rpms; 10 minutes time, collect supernatant.Throw out is added new extracting solution repeat aforesaid operations 3 times, merge supernatant, transfer pH8～9 with strong aqua; Place extractor with the ETHYLE ACETATE of 1/2 volume, stir extraction 15 minutes, left standstill 10 minutes; Is that 30 ℃, negative pressure are that the solvent thickener of 0.1MPa reclaims ETHYLE ACETATE with acetic acid ethyl acetate extract through temperature; Extraction liquid is concentrated into dried, after crystallization and purification on normal-phase silica gel column chromatography for separation, obtains the trimethyl-xanthine 3.08g of purity 92.3 again through recrystallization.
Claims (5)
1. method of from green tea, extracting trimethyl-xanthine, it is characterized in that: concrete steps are following: (1) with green tea, extract solution and add simultaneously and carry out homogenate in the refiner, with 0.5～5% aqueous sulfuric acid the pH value of homogenate is transferred to 2～3.5 then; Said extraction solution is the mixing solutions of aqueous sulfuric acid and inorganic salt solution, and wherein the pH of mixing solutions is 2～3.5, and the volumetric molar concentration of inorganic salt is 1M～3M; (2) use the ultrasonic extraction machine with the ultrasonication homogenate of frequency as 20KHz～1MHz; (3) adopt the centrifugal solid matter of removing of settling centrifuge to obtain extracting solution, rotating speed is 1000～6000 rpms, 3～20 minutes time; (4) with strong aqua the pH value of extracting solution is transferred to 8～11, extract with organic solvent then; (5) extraction liquid is concentrated into the dried trimethyl-xanthine mixture that obtains under 35～50 ℃ of temperature, negative pressure 0.07～0.1MPa or normal pressure; (6) with normal phase silicagel column the trimethyl-xanthine mixture is carried out purifying, used elutriant is the chloroform soln that contains 3～10% methyl alcohol; Carry out wash-out with elutriant, merge the elutriant that contains trimethyl-xanthine then, obtain the trimethyl-xanthine bullion at 35～50 ℃ of temperature, negative pressure 0.06～0.1MPa condition recover solvent; (7) gained trimethyl-xanthine bullion is carried out recrystallization and promptly get the trimethyl-xanthine product.
2. the method for from green tea, extracting trimethyl-xanthine according to claim 1 is characterized in that: said inorganic salt are a kind of or mixing more than two kinds wherein of sodium-chlor, Repone K, sodium sulfate or vitriolate of tartar.
3. the method for from green tea, extracting trimethyl-xanthine according to claim 1, it is characterized in that: the time of said ultrasonication homogenate is 10～90 minutes.
4. the method for from green tea, extracting trimethyl-xanthine according to claim 1, it is characterized in that: said organic solvent is an ETHYLE ACETATE.
5. the method for from green tea, extracting trimethyl-xanthine according to claim 1, it is characterized in that: used recrystallization solvent is 85%～95% ethanolic soln.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104032099A CN102516245A (en) | 2011-11-25 | 2011-11-25 | Method for extracting caffeine from green tea |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011104032099A CN102516245A (en) | 2011-11-25 | 2011-11-25 | Method for extracting caffeine from green tea |
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| CN102516245A true CN102516245A (en) | 2012-06-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875691A (en) * | 2012-10-19 | 2013-01-16 | 黄冈师范学院 | Method for synchronously preparing active substances from tea dregs |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875691A (en) * | 2012-10-19 | 2013-01-16 | 黄冈师范学院 | Method for synchronously preparing active substances from tea dregs |
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Application publication date: 20120627 |