CN107721965A - The extraction process of litchi rind OPC - Google Patents
The extraction process of litchi rind OPC Download PDFInfo
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- CN107721965A CN107721965A CN201711040011.2A CN201711040011A CN107721965A CN 107721965 A CN107721965 A CN 107721965A CN 201711040011 A CN201711040011 A CN 201711040011A CN 107721965 A CN107721965 A CN 107721965A
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- Prior art keywords
- ethanol
- litchi rind
- opc
- extraction process
- volumetric concentration
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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 OPC, comprise the following steps：1) litchi rind is smashed to pieces, adds ethanol solution extraction, obtain ethanol extract；2) ethanol extract is filtered, by filtrate recycling ethanol, obtains medicinal extract；3) it is that 50~70% ethanol solutions adjust litchi rind concentration to 0.3~0.5mg/ml that volumetric concentration is added into medicinal extract, stirring and dissolving, the upper macroreticular resins of XAD 7, first with distillation washing post, eluted again with the ethanol solution that volumetric concentration is 70~90%, collect efflux and ethanol eluate respectively；4) by AB 8+ resins on efflux, post first is washed with distillation, then is eluted with the ethanol solution that volumetric concentration is 40~50%, collects ethanol eluate；5) ethanol eluate will merge twice, filtering, filtrate concentration, freeze-drying, as litchi rind OPC.OPC 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 lichee peel anthocyanidin.
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.Contain a certain amount of OPC in lichee pericarp, OPC has very strong to free radical
Elimination ability is caught, is a kind of good oxygen free radical scavenger, has and suppresses erythrocyte membrane and low-density lipoprotein lipid mistake
Aoxidize, prevent platelet aggregation, prevent the functions such as cardiovascular and cerebrovascular disease, enjoy U.S. of " skin vitamin " and " oral cosmetic product "
Reputation.Prior art is less to the Study on extraction of lichee peel anthocyanidin, such as《The extraction of litchi rind OPC, purifying and oxidation
Activity research》(Zhou Weijing, Sun Zhida, Xie Bijun, Yang Erning, Food Science, on November 30th, 2009) discloses litchi rind original
The extraction process of anthocyanidin, first smashs lichee pericarp to pieces, weighs litchi rind raw material and is put in round-bottomed flask, adds ethanol, constant temperature
Water-bath, obtain extract solution；Extract solution is filtered, ethanol is recovered under reduced pressure with Rotary Evaporators, AB-8 macroporous absorbent resins in aqueous phase,
Using the distilled water and 50% ethanol stepwise elution of 10 times of amounts, ethanol eluate is concentrated in vacuo, is freeze-dried, obtains former cyanine
Element.After measured, the purity of OPC is 87.45%, yield 1.3%.
The content of the invention
High, the extraction work of the big litchi rind OPC 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 OPC, is comprised the following steps：
1) litchi rind is smashed to pieces, adds ethanol solution extraction, obtain ethanol extract；
2) ethanol extract is filtered, by filtrate recycling ethanol, obtains medicinal extract；
3) it is that 50~70% ethanol solutions adjust litchi rind concentration to 0.3~0.5mg/ that volumetric concentration is added into medicinal extract
Ml, stirring and dissolving, upper XAD-7 macroreticular resins, post first is washed with distillation, then washed with the ethanol solution that volumetric concentration is 70~90%
It is de-, efflux and ethanol eluate are collected respectively；
4) by AB-8+ resins on efflux, first with distillation washing post, then with the ethanol solution that volumetric concentration is 40~50%
Elution, collect ethanol eluate；
5) ethanol eluate will merge twice, filtering, filtrate concentration, freeze-drying, as litchi rind OPC.
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 1：30~50g/ml；Extracting temperature is 30~40 DEG C, is carried
It is 60~120min to take the time.
In step 3), 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 3), it is polar resin in 2- methacrylate types to select XAD-7 macroreticular resins, and average pore size is 0.8 μ
M, specific surface area are 450 ㎡/g.Because the high OPC of the degree of polymerization in litchi rind contains more phenolic hydroxyl group, polarity is higher,
It is similar to middle polar resin polarity, help to adsorb.Secondly, the resin can form weak hydrogen bond with phenolic hydroxyl group so that high polymerization degree
OPC be adsorbed on resin.Because aperture is larger, when using volumetric concentration as 70~90% ethanol solution elution,
Preferably the OPC of high polymerization degree can be eluted.
In step 4), 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 4), the AB-8+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：Milky spherical particle；
Specific surface area：520~550 ㎡/g；
Particle size range：0.3~1.2mm；
Average pore size：11.0~12.0nm；
Wet apparent density：0.7g/ml；
Porosity：45~50%；
Organic substance residues amount：≤20ppm.
AB-8+ macroreticular resins are applicants according to produce reality demand, are found by substantial amounts of experiment former AB-8 types is big
Hole resin average pore size change it is smaller, make its preferably by and adsorb litchi rind OPC oligomer, and macromolecule
Flavones and glycoside material, polysaccharide and protein substance then cannot be introduced into resin, and these macromolecular substances are direct without absorption
Outflow；And the material such as minimum carbohydrate of molecular weight is then passed through because molecular weight is too small by the speed of resin than OPC oligomer
The speed of resin is fast so that the macroreticular resin after improvement can be very good to adsorb OPC oligomer.In addition, AB-8+ is big
After hole resin aperture diminishes, specific surface area accordingly increases, and can increase adsorption area, and adsorption and desorption power increases so that former
Anthocyanidin separates more thoroughly with other impurities, improves purity and yield.
Compared with prior art, the invention has the advantages that：
1) polarity XAD-7 types resin can isolate and purify the OPC of high polymerization degree during the present invention first uses, then adopt
The OPC of low polymerization degree can be isolated and purified with AB-8+ types resin, can not only improve the yield of OPC, also greatly
Improve purity greatly.
2) present invention process is simple, and cost is cheap, is adapted to large-scale industrial production, and manufactured litchi rind OPC is received
Rate is high, and purity is big, high purity more than 96.0%, and high income is up to more than 1.8%.
Embodiment
The present invention is further elaborated for specific examples below, but not as a limitation of the invention.
Embodiment 1
1) litchi rind is smashed to pieces, adds the ethanol solution that volumetric concentration is 50% and extract, the material of litchi rind and ethanol solution
Liquor ratio is 1：30g/ml, 60min is extracted at 30 DEG C, obtains ethanol extract；
2) ethanol extract is filtered, by filtrate recycling ethanol, obtains medicinal extract；
3) it is that 50% ethanol solution adjusts litchi rind concentration to 0.3mg/ml that volumetric concentration is added into medicinal extract, is stirred molten
Solution, upper XAD-7 macroreticular resins, loading flow velocity is 8BV/h, and first with distillation washing post, the elution flow rate of distilled water is 15BV/h, then
Eluted with the ethanol solution that volumetric concentration is 70%, ethanol elution flow velocity is 10BV/h, collects efflux and ethanol elution respectively
Liquid；
4) by AB-8+ resins on efflux, loading flow velocity is 8BV/h, first with distillation washing post, the elution flow rate of distilled water
For 15BV/h, then eluted with the ethanol solution that volumetric concentration is 40%, ethanol elution flow velocity be 10BV/h, collection ethanol elution
Liquid；
The AB-8+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：Milky spherical particle；
Specific surface area：520~550 ㎡/g；
Particle size range：0.3~1.2mm；
Average pore size：11.0~12.0nm；
Wet apparent density：0.7g/ml；
Porosity：45~50%；
Organic substance residues amount：≤20ppm.
5) ethanol eluate will merge twice, filtering, filtrate concentration, freeze-drying, as litchi rind OPC.
It is using the purity and yield of sulfuric acid-vanillin method measure litchi rind OPC, purity 96.25%, yield
1.82%.
Embodiment 2
1) litchi rind is smashed to pieces, adds the ethanol solution that volumetric concentration is 70% and extract, the material of litchi rind and ethanol solution
Liquor ratio is 1：50g/ml, 120min is extracted at 40 DEG C, obtains ethanol extract；
2) ethanol extract is filtered, by filtrate recycling ethanol, obtains medicinal extract；
3) it is that 70% ethanol solution adjusts litchi rind concentration to 0.5mg/ml that volumetric concentration is added into medicinal extract, is stirred molten
Solution, upper XAD-7 macroreticular resins, loading flow velocity is 16BV/h, and first with distillation washing post, the elution flow rate of distilled water is 25BV/h,
Eluted again with the ethanol solution that volumetric concentration is 90%, ethanol elution flow velocity is 20BV/h, collects efflux respectively and ethanol is washed
De- liquid；
4) by AB-8+ resins on efflux, loading flow velocity is 16BV/h, first with distillation washing post, the elution stream of distilled water
Speed is 25BV/h, then is eluted with the ethanol solution that volumetric concentration is 50%, and ethanol elution flow velocity is 20BV/h, collects ethanol elution
Liquid；
The AB-8+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：Milky spherical particle；
Specific surface area：520~550 ㎡/g；
Particle size range：0.3~1.2mm；
Average pore size：11.0~12.0nm；
Wet apparent density：0.7g/ml；
Porosity：45~50%；
Organic substance residues amount：≤20ppm.
5) ethanol eluate will merge twice, filtering, filtrate concentration, freeze-drying, as litchi rind OPC.
It is using the purity and yield of sulfuric acid-vanillin method measure litchi rind OPC, purity 96.18%, yield
1.80%.
Embodiment 3
1) litchi rind is smashed to pieces, adds the ethanol solution that volumetric concentration is 60% and extract, the material of litchi rind and ethanol solution
Liquor ratio is 1：40g/ml, 100min is extracted at 35 DEG C, obtains ethanol extract；
2) ethanol extract is filtered, by filtrate recycling ethanol, obtains medicinal extract；
3) it is that 60% ethanol solution adjusts litchi rind concentration to 0.4mg/ml that volumetric concentration is added into medicinal extract, is stirred molten
Solution, upper XAD-7 macroreticular resins, loading flow velocity is 12BV/h, and first with distillation washing post, the elution flow rate of distilled water is 20BV/h,
Eluted again with the ethanol solution that volumetric concentration is 80%, ethanol elution flow velocity is 15BV/h, collects efflux respectively and ethanol is washed
De- liquid；
4) by AB-8+ resins on efflux, loading flow velocity is 10BV/h, first with distillation washing post, the elution stream of distilled water
Speed is 20BV/h, then is eluted with the ethanol solution that volumetric concentration is 45%, and ethanol elution flow velocity is 18BV/h, collects ethanol elution
Liquid；
The AB-8+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：Milky spherical particle；
Specific surface area：520~550 ㎡/g；
Particle size range：0.3~1.2mm；
Average pore size：11.0~12.0nm；
Wet apparent density：0.7g/ml；
Porosity：45~50%；
Organic substance residues amount：≤20ppm.
5) ethanol eluate will merge twice, filtering, filtrate concentration, freeze-drying, as litchi rind OPC.
It is using the purity and yield of sulfuric acid-vanillin method measure litchi rind OPC, purity 97.09%, yield
1.80%.
Embodiment 4
1) litchi rind is smashed to pieces, adds the ethanol solution that volumetric concentration is 50% and extract, the material of litchi rind and ethanol solution
Liquor ratio is 1：50g/ml, 120min is extracted at 30 DEG C, obtains ethanol extract；
2) ethanol extract is filtered, by filtrate recycling ethanol, obtains medicinal extract；
3) it is that 50% ethanol solution adjusts litchi rind concentration to 0.5mg/ml that volumetric concentration is added into medicinal extract, is stirred molten
Solution, upper XAD-7 macroreticular resins, loading flow velocity is 8BV/h, and first with distillation washing post, the elution flow rate of distilled water is 25BV/h, then
Eluted with the ethanol solution that volumetric concentration is 70%, ethanol elution flow velocity is 20BV/h, collects efflux and ethanol elution respectively
Liquid；
4) by AB-8+ resins on efflux, loading flow velocity is 8BV/h, first with distillation washing post, the elution flow rate of distilled water
For 25BV/h, then eluted with the ethanol solution that volumetric concentration is 40%, ethanol elution flow velocity be 20BV/h, collection ethanol elution
Liquid；
The AB-8+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：Milky spherical particle；
Specific surface area：520~550 ㎡/g；
Particle size range：0.3~1.2mm；
Average pore size：11.0~12.0nm；
Wet apparent density：0.7g/ml；
Porosity：45~50%；
Organic substance residues amount：≤20ppm.
5) ethanol eluate will merge twice, filtering, filtrate concentration, freeze-drying, as litchi rind OPC.
It is using the purity and yield of sulfuric acid-vanillin method measure litchi rind OPC, purity 96.33%, yield
1.84%.
Claims (6)
1. the extraction process of litchi rind OPC, it is characterised in that：Comprise the following steps：
1) litchi rind is smashed to pieces, adds ethanol solution extraction, obtain ethanol extract；
2) ethanol extract is filtered, by filtrate recycling ethanol, obtains medicinal extract；
3) it is that 50~70% ethanol solutions adjust litchi rind concentration to 0.3~0.5mg/ml that volumetric concentration is added into medicinal extract, is stirred
Dissolving is mixed, upper XAD-7 macroreticular resins, first washes post with distillation, then is eluted with the ethanol solution that volumetric concentration is 70~90%, point
Shou Ji not efflux and ethanol eluate；
4) by AB-8+ resins on efflux, post first is washed with distillation, then washed with the ethanol solution that volumetric concentration is 40~50%
It is de-, collect ethanol eluate；
5) ethanol eluate will merge twice, filtering, filtrate concentration, freeze-drying, as litchi rind OPC.
2. the extraction process of litchi rind OPC 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 OPC according to claim 1, it is characterised in that：In step 1), litchi rind
Solid-liquid ratio with ethanol solution is 1：30~50g/ml；Extracting temperature is 30~40 DEG C, and extraction time is 60~120min.
4. the extraction process of litchi rind OPC according to claim 1, it is characterised in that：In step 3), 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 OPC according to claim 1, it is characterised in that：In step 4), 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.
6. the extraction process of litchi rind OPC according to claim 1, it is characterised in that：In step 4), the AB-
8+ resins are polystyrene type nonpolar adsorption resin, and quality index is as follows：
Outward appearance：Milky spherical particle；
Specific surface area：520~550 ㎡/g；
Particle size range：0.3~1.2mm；
Average pore size：11.0~12.0nm；
Wet apparent density：0.7g/ml；
Porosity：45~50%；
Organic substance residues amount：≤20ppm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108850125A (en) * | 2018-09-03 | 2018-11-23 | 河南牧业经济学院 | A kind of cold antistaling beef agent |
| CN112159382A (en) * | 2020-09-14 | 2021-01-01 | 华南农业大学 | Method for efficiently preparing active oligomeric proanthocyanidins from physiological fruit drop of litchi |
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| CN102898411A (en) * | 2011-07-27 | 2013-01-30 | 周奕彤 | Proanthocyanidin extraction technology |
| CN104557838A (en) * | 2014-12-11 | 2015-04-29 | 惠州学院 | Method for extracting proantho cyanidins from litchi peels |
| CN105061529A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Extraction process of mulberry anthocyanin |
| 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 |
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2017
- 2017-10-31 CN CN201711040011.2A patent/CN107721965A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898411A (en) * | 2011-07-27 | 2013-01-30 | 周奕彤 | Proanthocyanidin extraction technology |
| CN104557838A (en) * | 2014-12-11 | 2015-04-29 | 惠州学院 | Method for extracting proantho cyanidins from litchi peels |
| CN105061529A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Extraction process of mulberry anthocyanin |
| 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 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108850125A (en) * | 2018-09-03 | 2018-11-23 | 河南牧业经济学院 | A kind of cold antistaling beef agent |
| CN112159382A (en) * | 2020-09-14 | 2021-01-01 | 华南农业大学 | Method for efficiently preparing active oligomeric proanthocyanidins from physiological fruit drop of litchi |
| CN112159382B (en) * | 2020-09-14 | 2023-02-28 | 华南农业大学 | Method for efficiently preparing active oligomeric proanthocyanidins from physiological fruit drop of litchi |
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