CN107722069A - The extraction process of litchi rind polyphenol - Google Patents
The extraction process of litchi rind polyphenol Download PDFInfo
- Publication number
- CN107722069A CN107722069A CN201711039922.3A CN201711039922A CN107722069A CN 107722069 A CN107722069 A CN 107722069A CN 201711039922 A CN201711039922 A CN 201711039922A CN 107722069 A CN107722069 A CN 107722069A
- Authority
- CN
- China
- Prior art keywords
- ethanol
- litchi rind
- polyphenol
- extraction process
- litchi
- Prior art date
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses the extraction process of litchi rind polyphenol, comprise the following steps：1) litchi rind is smashed to pieces, the ethanol solution that addition adjusts PH≤6.0 with hydrochloric 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 extraction process of litchi rind polyphenol.
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 extraction process of the big litchi rind polyphenol of yield the technical problem to be solved in the present invention is to provide a kind of purity.
Technical scheme provided by the invention is the extraction process of litchi rind polyphenol, is comprised the following steps：
1) litchi rind is smashed to pieces, the ethanol solution that addition adjusts PH≤6.0 with hydrochloric acid is extracted, and obtains ethanol extraction
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%.
Hydrochloric 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 is smashed to pieces, the volumetric concentration that addition adjusts PH 6.0 with hydrochloric acid is carried for 50% ethanol solution
Take, 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 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 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 is smashed to pieces, the volumetric concentration that addition adjusts PH 5.0 with hydrochloric acid is carried for 70% ethanol solution
Take, 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 and carry
Take 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 is smashed to pieces, the volumetric concentration that addition adjusts PH 4.0 with hydrochloric acid is carried for 60% ethanol solution
Take, 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 and carry
Take 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, the volumetric concentration that addition adjusts PH 2.0 with hydrochloric acid is carried 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 extraction process of litchi rind polyphenol, it is characterised in that：Comprise the following steps：
1) litchi rind is smashed to pieces, the ethanol solution that addition adjusts PH≤6.0 with hydrochloric 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 extraction process of litchi rind polyphenol according to claim 1, it is characterised in that：In step 1), ethanol solution
Volumetric concentration is 50~70%.
3. the extraction process of litchi rind polyphenol according to claim 1, it is characterised in that：In step 1), litchi rind and second
The solid-liquid ratio of alcoholic 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 polyphenol according to claim 1, it is characterised in that：In step 2), loading flow velocity is 8
~16BV/h, 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 polyphenol according to claim 1, it is characterised in that：In step 2), the D-101+
Resin is 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711039922.3A CN107722069A (en) | 2017-10-31 | 2017-10-31 | The extraction process of litchi rind polyphenol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711039922.3A CN107722069A (en) | 2017-10-31 | 2017-10-31 | The extraction process of litchi rind polyphenol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107722069A true CN107722069A (en) | 2018-02-23 |
Family
ID=61202961
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711039922.3A Pending CN107722069A (en) | 2017-10-31 | 2017-10-31 | The extraction process of litchi rind polyphenol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107722069A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013149323A1 (en) * | 2012-04-02 | 2013-10-10 | Ntegrity | Natural products for skin care |
| 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 |
| CN104547204A (en) * | 2014-12-11 | 2015-04-29 | 惠州学院 | Method for extracting polyphenol substances from litchi pericarp |
| CN104922271A (en) * | 2015-05-27 | 2015-09-23 | 广西壮族自冶区中国科学院广西植物研究所 | Application of litchi peel polyphenol in preparing drug or healthcare product for reducing liver cholesterol |
| CN105055669A (en) * | 2015-09-10 | 2015-11-18 | 桂林医学院 | Method for extracting polyphenol from golden camellia tea leaves |
| CN105687441A (en) * | 2016-04-01 | 2016-06-22 | 广西壮族自治区中国科学院广西植物研究所 | Application of litchi rind polyphenol in medicines for treating hyperglycemia and insulin resistance |
-
2017
- 2017-10-31 CN CN201711039922.3A patent/CN107722069A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013149323A1 (en) * | 2012-04-02 | 2013-10-10 | Ntegrity | Natural products for skin care |
| 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 |
| CN104547204A (en) * | 2014-12-11 | 2015-04-29 | 惠州学院 | Method for extracting polyphenol substances from litchi pericarp |
| CN104922271A (en) * | 2015-05-27 | 2015-09-23 | 广西壮族自冶区中国科学院广西植物研究所 | Application of litchi peel polyphenol in preparing drug or healthcare product for reducing liver cholesterol |
| CN105055669A (en) * | 2015-09-10 | 2015-11-18 | 桂林医学院 | Method for extracting polyphenol from golden camellia tea leaves |
| CN105687441A (en) * | 2016-04-01 | 2016-06-22 | 广西壮族自治区中国科学院广西植物研究所 | Application of litchi rind polyphenol in medicines for treating hyperglycemia and insulin resistance |
Non-Patent Citations (1)
| Title |
|---|
| 熊何健等，: ""荔枝多酚柱层析纯化工艺条件研究"", 《江西农业大学学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100537586C (en) | Method for producing high purity jasminoidin and high color number gardenia yellow pigment | |
| CN103626814A (en) | Method for separating anthocyanins monomer from lycium ruthenicum fruits | |
| CN103265519B (en) | The method of Folium Myricae rubrae proanthocyanidin is prepared in a kind of separation | |
| CN108558971A (en) | A kind of preparation method of roselle anthocyanin | |
| CN101863938A (en) | Method for preparing high-purity aucubin | |
| CN103980121B (en) | Method for producing chlorogenic acids from fresh eucommia leaves | |
| CN106588616A (en) | Preparation method of curcumin | |
| CN103450703A (en) | Method for preparing high-purity taste-removing purple sweet potato pigment | |
| CN102961486B (en) | Extraction method of longan seed polyphenol | |
| CN104910223A (en) | Preparation method of oleuropein | |
| CN103479751B (en) | Method for combined extraction of tritepenoidic acid, polyphenols and polysaccharides in loquat flower | |
| CN104356105B (en) | A kind of preparation method of EGCG | |
| CN107556284A (en) | The method that OPC is extracted from litchi rind | |
| CN101492350B (en) | Method for producing D-pinit from plant locust | |
| CN104926719A (en) | Method for extracting gynesine from fructus cannabis | |
| CN108003211A (en) | A kind of method of quick separating ganoderic acid in accessory substance from ganoderma lucidum | |
| CN107722069A (en) | The extraction process of litchi rind polyphenol | |
| CN103601771A (en) | Method for separating and preparing anthocyanin monomer from Nitraria tangutorum Bobr | |
| CN107773607A (en) | The method that litchi rind polyphenol is extracted from litchi rind | |
| CN104257701B (en) | A kind of method for preparing ganoderma lucidum triterpene compounds | |
| CN105503981A (en) | Method for extracting and separating anthocyanin from red cabbage | |
| CN105616477A (en) | Method for purifying polyphenol in lonicera edulis | |
| CN107721965A (en) | The extraction process of litchi rind OPC | |
| CN104230871A (en) | Method for separating polymethoxylated flavones, hesperidin and synephrine from immature bitter orange | |
| CN109320576A (en) | A kind of production method of high-content momordica grosvenori glycoside V |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180223 |
|
| WD01 | Invention patent application deemed withdrawn after publication |