CN107805236A - The extraction process of litchi rind epicatechin - Google Patents
The extraction process of litchi rind epicatechin Download PDFInfo
- Publication number
- CN107805236A CN107805236A CN201711053779.3A CN201711053779A CN107805236A CN 107805236 A CN107805236 A CN 107805236A CN 201711053779 A CN201711053779 A CN 201711053779A CN 107805236 A CN107805236 A CN 107805236A
- Authority
- CN
- China
- Prior art keywords
- ethanol
- litchi rind
- epicatechin
- extraction process
- litchi
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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 discloses the extraction process of litchi rind epicatechin, comprise the following steps：1) litchi rind is smashed to pieces, the ethanol solution that addition adjusts pH2.0~5.0 with sulfuric acid is extracted, and obtains ethanol extract；2) by CAD 40+ macroreticular resins on ethanol extract, post first is washed with distillation, then is eluted with the ethanol solution that volumetric concentration is 50~70%, collects ethanol eluate；3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind epicatechin.Litchi rind epicatechin purity produced by the present invention is high, and yield is big.
Description
Technical field
The present invention relates to technical field of biological extraction, and in particular to the extraction process of litchi rind epicatechin.
Background technology
Lichee is the fruit of sapindaceous plant lichee, is south China local product fruits.It is main in the industrialized production of lichee
Will be based on fresh fruit, dry fruit, can and dried product, and a large amount of litchi rinds are not developed effectively as accessory substance and profit
With usually as discarded object discarding.Litchi rind is rich in polyphenol components, predominantly epicatechin, rutin, forulic acid etc., has
The bioactivity such as anti-oxidant, anti-inflammatory, antitumor, there is exploitation profit well in fields such as functional food, health products, medicine bioengineerings
With value.Wherein, epicatechin is 3- hydroxyl flavane 01 derivatives, has the polyatomic phenol material of C6-C3-C6 structures, its base
This structure is α-phenyl benzopyrane, i.e., is connected between two phenyl ring with three carbochains, on one of carbon atom and A rings
Oxygen atom connect into pyranoid ring.Relevant report appearance is had not yet to see for extracting epicatechin from litchi rind.
The content of the invention
High, the extraction work of the big litchi rind epicatechin of yield the technical problem to be solved in the present invention is to provide a kind of purity
Skill.
Technical scheme provided by the invention is the extraction process of litchi rind epicatechin, is comprised the following steps：
1) litchi rind is smashed to pieces, the ethanol solution that addition adjusts pH2.0~5.0 with sulfuric acid is extracted, and is obtained ethanol and is carried
Take liquid；
2) first with distillation washing post, then with volumetric concentration it is 50~70% by CAD-40+ macroreticular resins on ethanol extract
Ethanol solution elution, collect ethanol eluate；
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind epicatechin.
In step 1), the volumetric concentration of ethanol solution is 50~70%.
In step 1), the solid-liquid ratio of litchi rind and ethanol solution is 1：15~25g/ml；Extracting temperature is 60~90 DEG C, is carried
It is 2~4h to take the time.
In step 2), loading flow velocity is 8~16BV/h, and the elution flow rate of distilled water is 15~25BV/h, ethanol elution stream
Speed is 10~20BV/h.
In step 2), the CAD-40+ resins are polystyrene type low pole polymeric adsorbent, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：55~65%；
Specific surface area：510~560 ㎡/g；
Particle size range：0.315~1.25mm >=90%；
Average pore size：4.5~5.0nm；
Wet apparent density：1.05~1.09g/ml；
Skeletal density：1.13~1.17g/ml.
CAD-40+ macroreticular resins are applicants according to produce reality demand, are found by substantial amounts of experiment by former CAD-40
Type macroreticular resin average pore size change it is smaller, make its preferably by and adsorb epicatechin, and the flavones of macromolecule, polysaccharide
Resin is then cannot be introduced into protein substance and rutin, these macromolecular substances flow directly out without absorption；And molecular weight
The materials such as minimum forulic acid are then faster by the speed of resin than epicatechin because of the too small speed by resin of molecular weight, make
Macroreticular resin after must improveing can be very good to adsorb epicatechin.In addition, after CAD-40+ macroreticular resins aperture diminishes, compare table
Area accordingly increases, and can increase adsorption area, and adsorption and desorption power increases so that small molecule free phenol and other impurities point
From more thoroughly, purity and yield are improved.
Compared with prior art, the invention has the advantages that：
1) present invention more preferably can will be separated epicatechin with impurity using CAD-40+ types resin, substantially increase table
The purity of catechin, yield also increase.
2) present invention process is simple, and cost is cheap, is adapted to large-scale industrial production, and manufactured litchi rind epicatechin is received
Rate is high, and purity is big, high purity more than 95.0%, and high income is up to more than 0.4%.
Embodiment
The present invention is further elaborated for specific examples below, but not as a limitation of the invention.
Embodiment 1
1) lichee dry hide to be smashed to pieces, the volumetric concentration that addition adjusts pH2.0 with sulfuric acid is extracted for 50% ethanol solution,
The solid-liquid ratio of litchi rind and ethanol solution is 1：15g/ml, Extracting temperature are 60 DEG C, extraction time 2h, obtain ethanol extraction
Liquid；
2) by CAD-40+ macroreticular resins on ethanol extract, loading flow velocity is 8BV/h, first with distillation washing post to outflow
Liquid is colourless, and the elution flow rate of distilled water is 15BV/h, then is eluted with the ethanol solution that volumetric concentration is 50%, ethanol elution flow velocity
For 10BV/h, ethanol eluate is collected；
The CAD-40+ macroreticular resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：55~65%；
Specific surface area：510~560 ㎡/g；
Particle size range：0.315~1.25mm >=90%；
Average pore size：4.5~5.0nm；
Wet apparent density：1.05~1.09g/ml；
Skeletal density：1.13~1.17g/ml；
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind epicatechin.
Using the purity and yield of F-C methods measure litchi rind lichee polyphenol, purity 96.07%, yield 0.42%.
Embodiment 2
1) lichee dry hide to be smashed to pieces, the volumetric concentration that addition adjusts pH5.0 with sulfuric acid is extracted for 70% ethanol solution,
The solid-liquid ratio of litchi rind and ethanol solution is 1：25g/ml, Extracting temperature are 90 DEG C, extraction time 4h, obtain ethanol extraction
Liquid；
2) by CAD-40+ macroreticular resins on ethanol extract, loading flow velocity is 16BV/h, first with distillation washing post to outflow
Liquid is colourless, and the elution flow rate of distilled water is 25BV/h, then is eluted with the ethanol solution that volumetric concentration is 70%, ethanol elution flow velocity
For 20BV/h, ethanol eluate is collected；
The CAD-40+ macroreticular resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：55~65%；
Specific surface area：510~560 ㎡/g；
Particle size range：0.315~1.25mm >=90%；
Average pore size：4.5~5.0nm；
Wet apparent density：1.05~1.09g/ml；
Skeletal density：1.13~1.17g/ml；
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind epicatechin.
Using the purity and yield of F-C methods measure litchi rind lichee polyphenol, purity 96.28%, yield 0.44%.
Embodiment 3
1) lichee dry hide to be smashed to pieces, the volumetric concentration that addition adjusts pH3.0 with sulfuric acid is extracted for 60% ethanol solution,
The solid-liquid ratio of litchi rind and ethanol solution is 1：20g/ml, Extracting temperature are 80 DEG C, extraction time 3h, obtain ethanol extraction
Liquid；
2) by CAD-40+ macroreticular resins on ethanol extract, loading flow velocity is 12BV/h, first with distillation washing post to outflow
Liquid is colourless, and the elution flow rate of distilled water is 20BV/h, then is eluted with the ethanol solution that volumetric concentration is 60%, ethanol elution flow velocity
For 15BV/h, ethanol eluate is collected；
The CAD-40+ macroreticular resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：55~65%；
Specific surface area：510~560 ㎡/g；
Particle size range：0.315~1.25mm >=90%；
Average pore size：4.5~5.0nm；
Wet apparent density：1.05~1.09g/ml；
Skeletal density：1.13~1.17g/ml；
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind epicatechin.
Using the purity and yield of F-C methods measure litchi rind lichee polyphenol, purity 95.76%, yield 0.43%.
Embodiment 4
1) lichee dry hide is smashed to pieces, addition is carried with the volumetric concentration of sulphur acid for adjusting pH 4.0 for 50% ethanol solution
Take, the solid-liquid ratio of litchi rind and ethanol solution is 1：25g/ml, Extracting temperature are 60 DEG C, extraction time 4h, obtain ethanol and carry
Take liquid；
2) by CAD-40+ macroreticular resins on ethanol extract, loading flow velocity is 8BV/h, first with distillation washing post to outflow
Liquid is colourless, and the elution flow rate of distilled water is 25BV/h, then is eluted with the ethanol solution that volumetric concentration is 50%, ethanol elution flow velocity
For 20BV/h, ethanol eluate is collected；
The CAD-40+ macroreticular resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：55~65%；
Specific surface area：510~560 ㎡/g；
Particle size range：0.315~1.25mm >=90%；
Average pore size：4.5~5.0nm；
Wet apparent density：1.05~1.09g/ml；
Skeletal density：1.13~1.17g/ml；
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind epicatechin.
Using the purity and yield of F-C methods measure litchi rind lichee polyphenol, purity 95.87%, yield 0.40%.
Claims (5)
1. the extraction process of litchi rind epicatechin, it is characterised in that：Comprise the following steps：
1) litchi rind is smashed to pieces, the ethanol solution that addition adjusts pH2.0~5.0 with sulfuric acid is extracted, and obtains ethanol extract；
2) by CAD-40+ macroreticular resins on ethanol extract, first with distillation washing post, then with the second that volumetric concentration is 50~70%
Alcoholic solution elutes, and collects ethanol eluate；
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind epicatechin.
2. the extraction process of litchi rind epicatechin according to claim 1, it is characterised in that：In step 1), ethanol is molten
The volumetric concentration of liquid is 50~70%.
3. the extraction process of litchi rind epicatechin according to claim 1, it is characterised in that：In step 1), litchi rind
Solid-liquid ratio with ethanol solution is 1：15~25g/ml；Extracting temperature is 60~90 DEG C, and extraction time is 2~4h.
4. the extraction process of litchi rind epicatechin according to claim 1, it is characterised in that：In step 2), loading stream
Speed is 8~16BV/h, and the elution flow rate of distilled water is 15~25BV/h, and ethanol elution flow velocity is 10~20BV/h.
5. the extraction process of litchi rind epicatechin according to claim 1, it is characterised in that：It is described in step 2)
CAD-40+ resins are polystyrene type low pole polymeric adsorbent, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：55~65%；
Specific surface area：510~560 ㎡/g；
Particle size range：0.315~1.25mm >=90%；
Average pore size：4.5~5.0nm；
Wet apparent density：1.05~1.09g/ml；
Skeletal density：1.13~1.17g/ml.
Priority Applications (1)
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| CN201711053779.3A CN107805236A (en) | 2017-10-31 | 2017-10-31 | The extraction process of litchi rind epicatechin |
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| CN201711053779.3A CN107805236A (en) | 2017-10-31 | 2017-10-31 | The extraction process of litchi rind epicatechin |
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| CN107805236A true CN107805236A (en) | 2018-03-16 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1733130A (en) * | 2005-09-01 | 2006-02-15 | 桂林莱茵生物科技股份有限公司 | Process for extracting litchi polyphenol from litchi |
| CN103908514A (en) * | 2014-04-25 | 2014-07-09 | 广西壮族自治区中国科学院广西植物研究所 | Process for extracting litchi polyphenol from litchi rind |
| CN105223300A (en) * | 2015-08-03 | 2016-01-06 | 广东药学院 | The method of quality control of lichee polyphenol and products thereof |
| CN106478580A (en) * | 2016-09-24 | 2017-03-08 | 合浦果香园食品有限公司 | A kind of method prepared from Fructus Litchi extract containing oligomeric proanthocyanidins |
-
2017
- 2017-10-31 CN CN201711053779.3A patent/CN107805236A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1733130A (en) * | 2005-09-01 | 2006-02-15 | 桂林莱茵生物科技股份有限公司 | Process for extracting litchi polyphenol from litchi |
| CN103908514A (en) * | 2014-04-25 | 2014-07-09 | 广西壮族自治区中国科学院广西植物研究所 | Process for extracting litchi polyphenol from litchi rind |
| CN105223300A (en) * | 2015-08-03 | 2016-01-06 | 广东药学院 | The method of quality control of lichee polyphenol and products thereof |
| CN106478580A (en) * | 2016-09-24 | 2017-03-08 | 合浦果香园食品有限公司 | A kind of method prepared from Fructus Litchi extract containing oligomeric proanthocyanidins |
Non-Patent Citations (2)
| Title |
|---|
| 夏涛等: "《茶叶深加工技术》", 28 February 2011, 中国轻工业出版社 * |
| 杨宏健: "《天然药物化学》", 31 August 2004, 郑州大学出版社 * |
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Application publication date: 20180316 |
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