CN107773607A - The method that litchi rind polyphenol is extracted from litchi rind - Google Patents
The method that litchi rind polyphenol is extracted from litchi rind Download PDFInfo
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- CN107773607A CN107773607A CN201711039958.1A CN201711039958A CN107773607A CN 107773607 A CN107773607 A CN 107773607A CN 201711039958 A CN201711039958 A CN 201711039958A CN 107773607 A CN107773607 A CN 107773607A
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- litchi rind
- ethanol
- polyphenol
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- litchi
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/77—Sapindaceae (Soapberry family), e.g. lychee or soapberry
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention discloses the method that litchi rind polyphenol is extracted from litchi rind, 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 D 101+ resins on ethanol extract, post first is washed with distillation, then is eluted with the ethanol solution that volumetric concentration is 40~50%, collects ethanol eluate；3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind polyphenol.Litchi rind polyphenol 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 method that litchi rind polyphenol is extracted from litchi rind.
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, mainly including free phenol, esterification phenol and insoluble phenol
Class, free phenol are water-soluble phenols, and esterification phenols is that phenolic compound is combined into carboxylate with cell wall polysaccharides and protein, and
Insoluble polyphenol is then the material that aldehydes matter is combined with compositions such as cell wall polysaccharides, and lichee polyphenol has anti-oxidant, anti-inflammatory, resisted
The bioactivity such as tumour, there is good value of exploiting and utilizing in fields such as functional food, health products, medicine bioengineerings.Publication number
CN103908514A patent of invention discloses the technique that lichee polyphenol is extracted from litchi rind, using litchi rind as raw material, first uses
PH≤6.0 of acid regulation extraction solvent, are then extracted to litchi rind with the solvent, degraded, gained extract solution crosses macropore tree
Fat post is adsorbed, model D-101, AB-8 of macroreticular resin, HPD100, HPD300, HPD700, H107, CAD-40,
D4020, HZ802, post is first washed with water, then washes post with low-carbon alcohols, thin-layer chromatography tracing detection, collect the alcohol containing target component and wash
De- liquid；Eluent is concentrated, dries, obtains lichee polyphenol.The litchi rind polyphenol purity that the above method obtains is 85%, and yield is only
For 1.0%.
The content of the invention
High the technical problem to be solved in the present invention is to provide a kind of purity, the big extraction litchi rind from litchi rind of yield is more
The method of phenol.
Technical scheme provided by the invention is the method that litchi rind polyphenol is extracted from litchi rind, 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) by D-101+ resins on ethanol extract, first with distillation washing post, then with the second that volumetric concentration is 40~50%
Alcoholic solution elutes, and collects ethanol eluate；
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind polyphenol.
In step 1), the volumetric concentration of ethanol solution is 50~70%.
Sulfuric acid regulation PH is added in Extraction solvent, can not only ensure that polyphenol is not oxidized, additionally aids esterification polyphenol
The free phenol of solubility is degraded into insoluble polyphenol.
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 D-101+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：65~75%；
Specific surface area：560~610 ㎡/g；
Particle size range：0.25~0.84mm；
Average pore size：8.5~9.0nm；
Wet apparent density：0.65~0.75g/ml.
D-101+ macroreticular resins are applicants according to produce reality demand, are found by substantial amounts of experiment by former D-101 types
Macroreticular resin average pore size change it is smaller, make its preferably by and adsorb the free polyphenol of small molecule, and the Huang of macromolecule
Ketone, polysaccharide and protein substance then cannot be introduced into resin, and these macromolecular substances flow directly out without absorption；And molecular weight pole
The materials such as small monose, polysaccharide are then fast by the speed of resin because of the too small speed specific ionization polyphenol by resin of molecular weight,
So that the macroreticular resin after improvement can be very good to adsorb free polyphenol.In addition, after D-101+ 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 small molecule polyphenol with impurity using D-101+ types resin, be substantially increased more
The purity of phenol, yield also increase.
2) present invention process is simple, and cost is cheap, is adapted to large-scale industrial production, manufactured litchi rind polyphenol yield
Height, purity is big, high purity more than 95.0%, and high income is up to more than 1.0%.
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 D-101+ resins on ethanol extract, loading flow velocity is 8BV/h, first with distillation washing post to efflux without
Color, the elution flow rate of distilled water is 15BV/h, then is eluted with the ethanol solution that volumetric concentration is 40%, and ethanol elution flow velocity is
10BV/h, collect ethanol eluate；
The D-101+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：65~75%；
Specific surface area：560~610 ㎡/g；
Particle size range：0.25~0.84mm；
Average pore size：8.5~9.0nm；
Wet apparent density：0.65~0.75g/ml.
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind polyphenol.
Using the purity and yield of F-C methods measure litchi rind lichee polyphenol, purity 95.43%, yield 1.25%.
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 D-101+ resins on ethanol extract, loading flow velocity is 16BV/h, first with distillation washing post to efflux without
Color, the elution flow rate of distilled water is 25BV/h, then is eluted with the ethanol solution that volumetric concentration is 50%, and ethanol elution flow velocity is
20BV/h, collect ethanol eluate；
The D-101+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：65~75%；
Specific surface area：560~610 ㎡/g；
Particle size range：0.25~0.84mm；
Average pore size：8.5~9.0nm；
Wet apparent density：0.65~0.75g/ml.
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind polyphenol.
Using the purity and yield of F-C methods measure litchi rind lichee polyphenol, purity 95.68%, yield 1.20%.
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 D-101+ resins on ethanol extract, loading flow velocity is 12BV/h, first with distillation washing post to efflux without
Color, the elution flow rate of distilled water is 20BV/h, then is eluted with the ethanol solution that volumetric concentration is 45%, and ethanol elution flow velocity is
15BV/h, collect ethanol eluate；
The D-101+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：65~75%；
Specific surface area：560~610 ㎡/g；
Particle size range：0.25~0.84mm；
Average pore size：8.5~9.0nm；
Wet apparent density：0.65~0.75g/ml.
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind polyphenol.
Using the purity and yield of F-C methods measure litchi rind lichee polyphenol, purity 95.18%, yield 1.30%.
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 D-101+ resins on ethanol extract, loading flow velocity is 8BV/h, first with distillation washing post to efflux without
Color, the elution flow rate of distilled water is 25BV/h, then is eluted with the ethanol solution that volumetric concentration is 40%, and ethanol elution flow velocity is
20BV/h, collect ethanol eluate；
The D-101+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：65~75%；
Specific surface area：560~610 ㎡/g；
Particle size range：0.25~0.84mm；
Average pore size：8.5~9.0nm；
Wet apparent density：0.65~0.75g/ml.
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind polyphenol.
Using the purity and yield of F-C methods measure litchi rind lichee polyphenol, purity 95.20%, yield 1.28%.
Claims (5)
1. the method for litchi rind polyphenol is extracted from litchi rind, 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 D-101+ resins on ethanol extract, post first is washed with distillation, then it is molten with the ethanol that volumetric concentration is 40~50%
Liquid elutes, and collects ethanol eluate；
3) ethanol eluate is filtered, filtrate concentration, freeze-drying, as litchi rind polyphenol.
2. the method according to claim 1 that litchi rind polyphenol is extracted from litchi rind, it is characterised in that：In step 1),
The volumetric concentration of ethanol solution is 50~70%.
3. the method according to claim 1 that litchi rind polyphenol is extracted from litchi rind, it is characterised in that：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, and extraction time is 2~4h.
4. the method according to claim 1 that litchi rind polyphenol is extracted from litchi rind, it is characterised in that：In step 2),
Loading flow velocity 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 method according to claim 1 that litchi rind polyphenol is extracted from litchi rind, it is characterised in that：In step 2),
The D-101+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：The opaque spherical particle of milky；
Moisture：65~75%；
Specific surface area：560~610 ㎡/g；
Particle size range：0.25~0.84mm；
Average pore size：8.5~9.0nm；
Wet apparent density：0.65~0.75g/ml.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711039958.1A CN107773607A (en) | 2017-10-31 | 2017-10-31 | The method that litchi rind polyphenol is extracted from litchi rind |
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| CN201711039958.1A CN107773607A (en) | 2017-10-31 | 2017-10-31 | The method that litchi rind polyphenol is extracted from litchi rind |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102895388A (en) * | 2012-09-28 | 2013-01-30 | 桂林益元素生物科技有限公司 | Lychee polyphenol extracts and extraction method thereof |
| WO2014059880A1 (en) * | 2012-10-18 | 2014-04-24 | 中国科学院新疆理化技术研究所 | Method for preparation of pomegranate-peel polyphenol gel used to treat gynecological inflammation |
| 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 |
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2017
- 2017-10-31 CN CN201711039958.1A patent/CN107773607A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102895388A (en) * | 2012-09-28 | 2013-01-30 | 桂林益元素生物科技有限公司 | Lychee polyphenol extracts and extraction method thereof |
| WO2014059880A1 (en) * | 2012-10-18 | 2014-04-24 | 中国科学院新疆理化技术研究所 | Method for preparation of pomegranate-peel polyphenol gel used to treat gynecological inflammation |
| 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 |
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Application publication date: 20180309 |