CN106854193A - A kind of preparation method that catechin is extracted from tealeaves - Google Patents
A kind of preparation method that catechin is extracted from tealeaves Download PDFInfo
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- CN106854193A CN106854193A CN201510898020.XA CN201510898020A CN106854193A CN 106854193 A CN106854193 A CN 106854193A CN 201510898020 A CN201510898020 A CN 201510898020A CN 106854193 A CN106854193 A CN 106854193A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
Abstract
The invention belongs to separation and extraction technology field, it is related to a kind of preparation method that catechin is extracted from tealeaves.The preparation method is comprised the following steps：By drying tea leaves, it is milled to Tea Samples；Tea Samples are weighed, ethanol solution is added, is placed in microwave dissolver and is extracted, filtration washing obtains extract solution；Extract solution addition chloroform is extracted into obtain the aqueous solution, then the aqueous solution is extracted with ethyl acetate, water phase is removed, ester mutually depressurizes Distillation recovery ethyl acetate, then catechin is obtained after vacuum concentration, freeze-drying and slightly carry product；Catechin is slightly carried product first through chromatograph pre-separation, then with preparation HPLC purify refine, obtain high-purity catechin.Operating procedure of the present invention is simple, and solvent load is few, and recovery rate is high, is suitable to laboratory and prepares on a small quantity, also can large-scale industrial production.
Description
Technical field
The invention belongs to separation and extraction technology field, it is related to a kind of preparation method that catechin is extracted from tealeaves.
Background technology
Tea Polyphenols is the general name of Polyphenols of Tea, mainly by the class material composition of catechin, flavonoids, anthocyanidin and phenolic acid etc. four, most important of which is that the flavanol compound based on catechin, its content accounts for Polyphenols total amount more than 70%, the health care of catechin and pharmacological function are summarized as Mao Qingli etc. " three anti-(anticancer, anti-aging, anti-oxidant) ", " three drops (hypoglycemic, reducing blood lipid, hypotensive) " and " three disappear (sterilization, anti-inflammatory, smelly eliminating) " (" tea catechin health care and pharmacological function New research progress ", Mao Qingli etc.《Food Science》, the 8th phase of volume 28, the 584-589 pages, in August, 2007), catechin is the important component of tea tree secondary metabolism, is also the important component of tea health-care effect, and the formation to the color quality of tealeaves plays an important role.
In the prior art, the conventional preparation method of catechin is extracted in tealeaves and mainly includes machine solvent extraction, supercritical fluid extraction, ion catch electron microscopy etc..Wherein, organic solvent extractionprocess is mainly in whole process using various organic solvents, and consumption of organic solvent is big, and operation is more, and technique is cumbersome, and active constituent content and recovery rate are low.The recovery rate that supercritical fluid extraction is mainly manifested in once is very low, while also relevant with other some factors such as flow velocitys of extraction time, fluid etc..Ion catch electron microscopy, pH value is adjusted because method precipitation turns molten, part catechin is already oxidised thus product colour is general deeper during this period, influence quality, due also to the limitation of extraction process, often impurity content is high in product, it is only rested on laboratory and prepares on a small quantity and be not easy to industrialized production, limits the popularization and application of tea extract.
The content of the invention
The purpose of the present invention is to overcome complex operation in the prior art, and solvent-oil ratio is big, and recovery rate is not high, is not easy to the problem of control of industrialization.Therefore, the invention provides a kind of preparation method that catechin is extracted from tealeaves.
The preparation method includes following technological process：
1）, raw material pre-treatment：Tealeaves is dried under conditions of 80~120 DEG C, Tea Samples are milled to；
2）, microwave radiation technology extraction：Tea Samples are weighed in polytetrafluoroethylene (PTFE) counteracting tank, it is 60% ~ 80% ethanol solution to add mass concentration, tightens tank mouth, is subsequently placed in microwave dissolver, carries out microwave digestion, filtering and concentrating filtrate；
3）, isolate and purify：Extract solution equal amounts of chloroform is extracted repeatedly, stratification, merge the aqueous solution, then the aqueous solution is extracted repeatedly with the ethyl acetate of equivalent, remove water phase, ester mutually depressurizes Distillation recovery ethyl acetate, then catechin is obtained after vacuum concentration, freeze-drying and slightly carry product；
4）, finished product processing：Catechin is slightly carried product first through chromatographing pre-separation, then purify refined, prepared high-purity catechin with preparation HPLC.
A kind of above-mentioned preparation method that catechin is extracted from tealeaves, described grinding was 80 mesh sieves.
A kind of above-mentioned preparation method that catechin is extracted from tealeaves, described microwave dissolver, setting power is 720 ~ 900 W, and the time is 5 ~ 7min, and temperature is 80~90 DEG C, and solid-liquid ratio is 1:80.
A kind of above-mentioned preparation method that catechin is extracted from tealeaves, described finished product processing is specific as follows shown：
Coarse extraction catechin 10g, it is dissolved in water to 100ml, filtering, upper Sephadex LH-20 posts, first eluted with pure water 500ml, be a unit stream part per 100ml then successively with the acetone gradient elution that 1000ml volume fractions are 30%, 45%, 60%, 80%, collect respectively and make HPLC analyses, catechin crude product obtains four kinds of stream parts：When being eluted with pure water and 30% acetone, outflow mainly contains the stream part one of caffeine material；Then non-ester catechin and ester catechin are separated, and the stream part two and stream part three for successively flowing out, wherein described non-ester catechin includes epigallocatechin EGC, catechin C and epicatechin EC, and the ester catechin includes Epigallo-catechin gallate (EGCG) EGCG, L-Epicatechin gallate ECG and nutgall catechin gallic acid ester GCG；Finally when being eluted with the acetone that volume fraction is 80%, outflow mainly contains the stream part four of pigment impurity.
Through chromatographing pre-separation, stream part one containing caffeine and the stream part containing coloring matter four are removed, merge stream part two and the concentrated removing acetone of stream part three, by the solution after concentrated removing acetone, with pure water and 80% methanol solution as eluent, and make HPLC analyses, stream part containing Epigallo-catechin gallate (EGCG) EGCG, nutgall catechin gallic acid ester GCG, L-Epicatechin gallate ECG respectively is merged, 40 DEG C of reduced vacuums reclaim eluting solvent, each catechin is obtained, gained catechin product purity is higher.
Beneficial effects of the present invention：By contrasting prior art, the present invention is extracted using microwave radiation technology, and its heating is fast, it is high to heat up, and clears up ability by force, and the solvent of consumption is few, reduces oxidation of the catechin when extracting, and extract quality is greatly improved；Catechin sterling is obtained with the refined method successive extract of multiple extraction, chromatography, HPLC, its method is simple to operate, and gained sample purity is high, it is easy to control of industrialization.
Specific embodiment
It is described in further detail below by embodiment.
Embodiment one
Tealeaves is dried under conditions of 80 DEG C, 80 mesh sieves into Tea Samples are crossed；100g Tea Samples are weighed in polytetrafluoroethylene (PTFE) counteracting tank, is 1 by solid-liquid ratio:80 ethanol solutions for adding mass concentration 60%, tighten tank mouth, are subsequently placed in microwave dissolver, and setting power is 720W, and the time is 5min, and temperature is 80 DEG C, carries out microwave digestion, then filtration washing, and ethanol is reclaimed in vacuum distillation, obtains extract solution；Extract solution equal amounts of chloroform is extracted repeatedly, stratification, merge the aqueous solution, then the aqueous solution is extracted repeatedly with the ethyl acetate of equivalent, remove water phase, ester mutually depressurizes Distillation recovery ethyl acetate, then catechin is obtained after vacuum concentration, freeze-drying and slightly carry product.Catechin is slightly carried product first through chromatographing pre-separation, HPLC purifying is refined specific as follows shown：
Coarse extraction catechin 10g, it is dissolved in water to 100ml, filtering, upper Sephadex LH-20 posts, are first eluted with pure water 500ml, then successively with acetone gradient elution that 1000ml volume fractions are 30%, 45%, 60%, 80%, it is a unit stream part per 100ml, collect in triangular flask respectively, HPLC analyses are then made to stream part in each bottle, catechin crude product obtains four kinds of stream parts：When being eluted with pure water and 30% acetone, outflow mainly contains the stream part one of caffeine material；Then non-ester catechin and ester catechin are separated, and the successively stream part two and stream part three of outflow；Wherein described non-ester catechin includes epigallocatechin EGC, catechin C and epicatechin EC, and the ester catechin includes Epigallo-catechin gallate (EGCG) EGCG, L-Epicatechin gallate ECG and nutgall catechin gallic acid ester GCG；Finally when being eluted with the acetone that volume fraction is 80%, outflow mainly contains the stream part four of pigment impurity.Through chromatographing pre-separation, stream part one containing caffeine and the stream part containing coloring matter four are removed, merge stream part two and the concentrated removing acetone of stream part three, by the solution after concentrated removing acetone, with pure water and 80% methanol solution as eluent, and make HPLC analyses, stream part containing Epigallo-catechin gallate (EGCG) EGCG, nutgall catechin gallic acid ester GCG, L-Epicatechin gallate ECG respectively is merged, 40 DEG C of reduced vacuums reclaim eluting solvent, each catechin is obtained, gained catechin product purity is higher.Load the moistureproof preservation of closed container lucifuge, it is standby.After testing, its purity is up to more than 90%.
Embodiment two
Tealeaves is dried under conditions of 90 DEG C, 80 mesh sieves into Tea Samples are crossed；100g Tea Samples are weighed in polytetrafluoroethylene (PTFE) counteracting tank, is 1 by solid-liquid ratio:80 ethanol solutions for adding mass concentration 70%, tighten tank mouth, are subsequently placed in microwave dissolver, and setting power is 800W, and the time is 6min, and temperature is 90 DEG C, carries out microwave digestion, then filtration washing, and ethanol is reclaimed in vacuum distillation, obtains extract solution；Extract solution equal amounts of chloroform is extracted repeatedly, stratification, merge the aqueous solution, then the aqueous solution is extracted repeatedly with the ethyl acetate of equivalent, remove water phase, ester mutually depressurizes Distillation recovery ethyl acetate, then catechin is obtained after vacuum concentration, freeze-drying and slightly carry product.Catechin is slightly carried product first through chromatography pre-separation, then is purified with preparation HPLC refined（With the corresponding steps of embodiment one）, high-purity catechin is obtained.Load the moistureproof preservation of closed container lucifuge, it is standby.After testing, its purity is up to more than 90%.
Embodiment three
Tealeaves is dried under conditions of 100 DEG C, 80 mesh sieves into Tea Samples are crossed；100g Tea Samples are weighed in polytetrafluoroethylene (PTFE) counteracting tank, is 1 by solid-liquid ratio:80 ethanol solutions for adding mass concentration 80%, tighten tank mouth, are subsequently placed in microwave dissolver, and setting power is 900W, and the time is 7min, and temperature is 100 DEG C, carries out microwave digestion, then filtration washing, and ethanol is reclaimed in vacuum distillation, obtains extract solution；Extract solution equal amounts of chloroform is extracted repeatedly, stratification, merge the aqueous solution, then the aqueous solution is extracted repeatedly with the ethyl acetate of equivalent, remove water phase, ester mutually depressurizes Distillation recovery ethyl acetate, then catechin is obtained after vacuum concentration, freeze-drying and slightly carry product.Catechin is slightly carried product first through chromatography pre-separation, then is purified with preparation HPLC refined（With the corresponding steps of embodiment one）, high-purity catechin is obtained.Load the moistureproof preservation of closed container lucifuge, it is standby.After testing, its purity is up to more than 90%.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert that specific implementation of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, should all be considered as belonging to protection scope of the present invention.
Claims (4)
1. it is a kind of from tealeaves extract catechin preparation method, it is characterised in that：The preparation method includes following technological process：
1）, raw material pre-treatment：Tealeaves is dried under conditions of 80~120 DEG C, Tea Samples are milled to；
2）, microwave radiation technology extraction：Tea Samples are weighed in polytetrafluoroethylene (PTFE) counteracting tank, it is 60% ~ 80% ethanol solution to add mass concentration, tightens tank mouth, is subsequently placed in microwave dissolver, carries out microwave digestion, then filtration washing, and ethanol is reclaimed in vacuum distillation, obtains extract solution；
3）, isolate and purify：Extract solution equal amounts of chloroform is extracted repeatedly, stratification, merge the aqueous solution, then the aqueous solution is extracted repeatedly with the ethyl acetate of equivalent, remove water phase, ester mutually depressurizes Distillation recovery ethyl acetate, then catechin is obtained after vacuum concentration, freeze-drying and slightly carry product；
4）, finished product processing：Catechin is slightly carried product first through chromatographing pre-separation, then purify refined, prepared high-purity catechin with preparation HPLC.
2. preparation method according to claim 1, it is characterised in that：Described grinding was 80 mesh sieves.
3. preparation method according to claim 1, it is characterised in that：Described microwave dissolver setting power is 720 ~ 900 W, and the time is 5 ~ 7min, and temperature is 80~90 DEG C, and solid-liquid ratio is 1:80.
4. preparation method according to claim 1, it is characterised in that：Shown in described finished product processing is specific as follows：
Coarse extraction catechin 10g, it is dissolved in water to 100ml, filtering, upper Sephadex LH-20 posts, first eluted with pure water 500ml, be a unit stream part per 100ml then successively with the acetone gradient elution that 1000ml volume fractions are 30%, 45%, 60%, 80%, collect respectively and make HPLC analyses, catechin crude product obtains four kinds of stream parts：
When being eluted with pure water and 30% acetone, outflow mainly contains the stream part one of caffeine material；Then non-ester catechin and ester catechin are separated, and the stream part two and stream part three for successively flowing out, wherein described non-ester catechin includes epigallocatechin EGC, catechin C and epicatechin EC, and the ester catechin includes Epigallo-catechin gallate (EGCG) EGCG, L-Epicatechin gallate ECG and nutgall catechin gallic acid ester GCG；Finally when being eluted with the acetone that volume fraction is 80%, outflow mainly contains the stream part four of pigment impurity；
Through chromatographing pre-separation, stream part one containing caffeine material and the stream part containing pigment impurity four are removed, merge stream part two and the concentrated removing acetone of stream part three, by the solution after concentrated removing acetone, with pure water and 80% methanol solution as eluent, and make HPLC analyses, stream part containing Epigallo-catechin gallate (EGCG) EGCG, nutgall catechin gallic acid ester GCG, L-Epicatechin gallate ECG respectively is merged, 40 DEG C of reduced vacuums reclaim eluting solvent, obtain each catechin.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957884A (en) * | 2016-01-12 | 2017-07-18 | 中华全国供销合作总社杭州茶叶研究所 | A kind of theaflavin product rich in tea catechin |
| CN109384762A (en) * | 2018-12-14 | 2019-02-26 | 成都华高生物制品有限公司 | The extracting method of ECG catechin in a kind of tealeaves |
| CN111838666A (en) * | 2020-08-10 | 2020-10-30 | 桑迪(武汉)生物科技有限公司 | Composition with auxiliary memory improving function and application thereof |
| CN111869769A (en) * | 2020-06-24 | 2020-11-03 | 浙江天草生物科技股份有限公司 | Production process of high-yield high-ester catechin green tea extract |
| CN113512020A (en) * | 2021-04-07 | 2021-10-19 | 湖南大学 | Method for extracting catechin and epicatechin from pericarp of plant of Camellia |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957884A (en) * | 2016-01-12 | 2017-07-18 | 中华全国供销合作总社杭州茶叶研究所 | A kind of theaflavin product rich in tea catechin |
| CN106957884B (en) * | 2016-01-12 | 2020-10-02 | 中华全国供销合作总社杭州茶叶研究所 | Theaflavin product rich in tea catechin |
| CN109384762A (en) * | 2018-12-14 | 2019-02-26 | 成都华高生物制品有限公司 | The extracting method of ECG catechin in a kind of tealeaves |
| CN111869769A (en) * | 2020-06-24 | 2020-11-03 | 浙江天草生物科技股份有限公司 | Production process of high-yield high-ester catechin green tea extract |
| CN111838666A (en) * | 2020-08-10 | 2020-10-30 | 桑迪(武汉)生物科技有限公司 | Composition with auxiliary memory improving function and application thereof |
| CN113512020A (en) * | 2021-04-07 | 2021-10-19 | 湖南大学 | Method for extracting catechin and epicatechin from pericarp of plant of Camellia |
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Application publication date: 20170616 |