CN106822315A - The method that flavones is extracted from pomelo peel - Google Patents
The method that flavones is extracted from pomelo peel Download PDFInfo
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- CN106822315A CN106822315A CN201710195440.0A CN201710195440A CN106822315A CN 106822315 A CN106822315 A CN 106822315A CN 201710195440 A CN201710195440 A CN 201710195440A CN 106822315 A CN106822315 A CN 106822315A
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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)
- A61K36/75—Rutaceae (Rue family)
- A61K36/752—Citrus, e.g. lime, orange or lemon
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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 belongs to the technical field of Nature inorganic bone, more particularly to a kind of method that flavones is extracted from pomelo peel, including following preparation process：1) pomelo peel drying is taken, is crushed；2) the pomelo peel high-speed shearing emulsion machine after crushing is processed；3) ultrasonic wave extraction；4) by flavones crude extract by macroporous adsorbent resin column chromatography, eluent is collected；5) eluent crosses different molecular weight hollow-fibre membrane；6) concentrate, dry, you can.Flavones is extracted from pomelo peel by the inventive method, it is possible to achieve turn waste into wealth, make full use of resource, and the flavones for preparing has high-purity and high extraction, while realizing that high-purity and high extraction are that present technology is extremely difficult to.
Description
Technical field
The invention belongs to the technical field of Nature inorganic bone, more particularly to a kind of method that flavones is extracted from pomelo peel.
Background technology
Shaddock also known as " pomelo ", crust is very thick, is plucked in 10~November mostly.Shaddock is more common in south, with Zhangzhou, Fujian,
It is the most famous that shaddock is produced in Xiamen.It is good to eat that its fruit eats sweet acid raw, refreshing, makes us being profuse in praise；Its pericarp, pomelo flower all may be used
It is used as medicine, there is the title of " natural fruit can ".The effects such as wherein pomelo peel has edible, dispelling odor, mosquito proof.Shaddock is not only sought
Support value high, but also with stomach invigorating, moistening lung, enrich blood, gut purge, it is convenient the effects such as, wound healing can be promoted, have to septicaemia etc.
Good auxiliary curative effect.Shaddock contains physiological activator skin glucoside, so the viscosity of blood can be reduced, reduces the shape of thrombus
Into, so to cranial vascular disease, such as cerebral thrombus, apoplexy also has preferable prevention effect.
Containing abundant aromatic oil, pectin, dietary fiber, pigment etc. in shaddock, also containing with resolving sputum antibechic, the treatment heart
The Flavonoid substances such as the aurantiin of the multiple efficacies such as cranial vascular disease.Wherein, Flavonoid substances belong to the active ingredient in shaddock.Shaddock
In in pericarp, Naringin Extracted from Pomelo Peel content is about 1%~6% to more than 50% Flavonoid substances point, mainly in son
Flavanone kind composition, such as aurantiamarin, neohesperidin, narirutin.
Used as the important industrial crops of south China, the annual yield of shaddock is up to 100,000 tons.Except edible pulp portion
Point, still there is the pericarp for accounting for fresh weight 20%~30% to utilize.The degraded of these agricultural wastes, on the one hand to the ecosystem
Stabilization produces huge pressure, on the other hand then wastes wherein substantial amounts of resource (such as flavonoids, pectin, dietary fiber).
Therefore, a kind of flavones that high-purity and high extraction are extracted from pomelo peel is researched and developed, strengthens the comprehensive utilization of pomelo peel, become
Waste be changed into values, improves its added value and is highly desirable to.
The content of the invention
The technical problems to be solved by the invention are to provide the method that flavones is extracted from pomelo peel, and the method is prepared
Flavones purity, recovery rate and bioactivity it is high.
To achieve the above object, technical scheme to be solved by this invention is：
The present invention provides the method that flavones is extracted from pomelo peel, including following preparation process：
1) pomelo peel drying is taken, is crushed；
2) by the pomelo peel after crushing according to 1:8~16 weight is than adding ethanol solution, high-speed shearing emulsion machine treatment
22~30min, rotating speed is 1800~2800r/min；
3) 15~28min of ultrasonic wave extraction under 35~85KHz frequencies, obtains flavones crude extract；
4) flavones crude extract is eluted by macroporous adsorbent resin column chromatography by eluant, eluent of ethanol solution, is collected
Eluent；
5) eluent crosses the hollow-fibre membrane that molecular cut off is 5~80,000, and permeate a and concentrate a is collected respectively；Will
Concentrate a crosses the hollow-fibre membrane that molecular cut off is 45~600,000, collects permeate b；Merge permeate a and permeate b；
6) concentrate, dry, you can.
In order that pomelo peel be easier to crush, step 1 of the present invention) in, pomelo peel dry to aqueous component be 30~
40%.
In order to accelerate the effective dissolution of the flavonoid substance in pomelo peel, while the bioactivity in order to improve flavones, the present invention
The step 1) in, it is crushed to 80~120 mesh.
Step 2 of the present invention) in, the volumetric concentration of ethanol solution is 65~75%.The volumetric concentration of solvent is suitable, energy
Enough flavones active principles extracted to greatest extent in pomelo peel, while avoiding concentration excessive, waste solvent, improve cost.
In order to the active principle for ensureing flavones is not destroyed, the active principle bioactivity of flavones is improved, it is of the present invention
Step 3) in, temperature during ultrasonic wave extraction is 35~55 DEG C, at such a temperature, most useful for the dissolution of flavones active principle, contracting
Short extraction time.
In order that flavonoid substance is eluted faster, while multi-solvent was not wasted, step 4 of the present invention) in, ethanol is molten
The addition of liquid is 2~6 times of resin volume.
Eluted under this volumetric concentration, the flavones active principle purity for preparing is higher, and wash-out is faster, the present invention
The step 4) in, the volumetric concentration of ethanol solution is 55~75%.
Step 4 of the present invention) in, ethanol solution is eluted with the flow velocity of 0.8~2.2BV/h, is washed in this flow velocity
De-, wash-out has optimum efficiency, if can cause production cycle process slowly excessively, efficiency is low, influence yield, and too fast flavonoid substance
Have little time just to be rushed out chromatographic column by macroporous resin adsorption, cause the waste of raw material, reduce recovery rate.
Step 6 of the present invention) in, the medicinal extract that relative density is 1.1~1.2 is concentrated at 35 DEG C.It is condensed into medicinal extract
Be conducive to drying below.
Step 6 of the present invention) in, freeze-drying is conducive to keeping the bioactivity of flavones.
The inventive method before extraction, is processed with high-speed shearing emulsion machine, raw material is constantly produced new interface, and material is cut
Disconnected, compression, fold, make its stirring, mixing and be downwardly toward at the homogenizer below pot, then rotor by high speed rotation with
The process such as cutting, dispersion, impact, sinuous flow of produced strength makes material be cut in seam is sheared between stator, rapid broken
Be broken into the particulate of 200nm~2 μm, make the continuous dissolution of flavones active ingredient, beneficial to the treatment of subsequent technique, beneficial to improve activity into
The yield for dividing, shortens extraction time.
The present invention carries out ultrasonication after being processed with high-speed shearing emulsion machine, mild condition, effectively prevent effectively into
Divide and be not destroyed, improve the bioactivity of flavones, and can to greatest extent extract flavones active ingredient, macroporous absorption tree is crossed afterwards
Fat column chromatography be conducive to improve flavones purity, then PSPP hollow-fibre membrane, can further improve purity,
And extract the flavones molecular weight that obtains between 5~80,000 and 45~600,000, the flavones in the interval range in digestive system not
Degradable, its molecule still keeps activated state, can still play original activity, by it is oral when, its anticancer effect is notable.
Flavones is extracted from pomelo peel by the inventive method, it is possible to achieve turn waste into wealth, make full use of resource, and prepare
The flavones for obtaining has high-purity and high extraction, while realizing that high-purity and high extraction are that present technology is extremely difficult to.
Specific embodiment
The invention will be further described with reference to embodiments, but the invention is not limited in these embodiments.
Embodiment 1
The method that flavones is extracted from pomelo peel, including following preparation process：
1) it is 30% to take pomelo peel and dry to aqueous component, is crushed to 120 mesh；
2) by the pomelo peel after crushing according to 1:8 weight is cut at a high speed than the ethanol solution for adding volumetric concentration to be 65%
Mulser treatment 22min is cut, rotating speed is 2800r/min；
3) the ultrasonic wave extraction 15min at a temperature of 35KHz frequencies and 55 DEG C, obtains flavones crude extract；
4) by flavones crude extract by macroporous adsorbent resin column chromatography, the volumetric concentration with 6 times of resin volume is 55%
Ethanol solution eluted for eluant, eluent, ethanol solution is eluted with the flow velocity of 2.2BV/h, collects eluent；
5) eluent crosses the hollow-fibre membrane that molecular cut off is 50,000, and permeate a and concentrate a is collected respectively；Will concentration
Liquid a crosses the hollow-fibre membrane that molecular cut off is 550,000, collects permeate b；Merge permeate a and permeate b；
6) medicinal extract that relative density is 1.1, freeze-drying are concentrated at 35 DEG C, you can.
Detected through HPLC, up to 99.3%, it is 94.2% to be computed recovery rate to flavones purity.
Embodiment 2
The method that flavones is extracted from pomelo peel, including following preparation process：
1) it is 35% to take pomelo peel and dry to aqueous component, is crushed to 110 mesh；
2) by the pomelo peel after crushing according to 1:10 weight is cut at a high speed than the ethanol solution for adding volumetric concentration to be 70%
Mulser treatment 24min is cut, rotating speed is 2500r/min；
3) the ultrasonic wave extraction 19min at a temperature of 45KHz frequencies and 50 DEG C, obtains flavones crude extract；
4) by flavones crude extract by macroporous adsorbent resin column chromatography, the volumetric concentration with 5 times of resin volume is 60%
Ethanol solution eluted for eluant, eluent, ethanol solution is eluted with the flow velocity of 1.9BV/h, collects eluent；
5) eluent crosses the hollow-fibre membrane that molecular cut off is 60,000, and permeate a and concentrate a is collected respectively；Will concentration
Liquid a crosses the hollow-fibre membrane that molecular cut off is 600,000, collects permeate b；Merge permeate a and permeate b；
6) medicinal extract that relative density is 1.12, freeze-drying are concentrated at 35 DEG C, you can.
Detected through HPLC, up to 99.6%, it is 95.1% to be computed recovery rate to flavones purity.
Embodiment 3
The method that flavones is extracted from pomelo peel, including following preparation process：
1) it is 40% to take pomelo peel and dry to aqueous component, is crushed to 100 mesh；
2) by the pomelo peel after crushing according to 1:12 weight is cut at a high speed than the ethanol solution for adding volumetric concentration to be 75%
Mulser treatment 26min is cut, rotating speed is 2300r/min；
3) the ultrasonic wave extraction 22min at a temperature of 55KHz frequencies and 45 DEG C, obtains flavones crude extract；
4) by flavones crude extract by macroporous adsorbent resin column chromatography, the volumetric concentration with 4 times of resin volume is 65%
Ethanol solution eluted for eluant, eluent, ethanol solution is eluted with the flow velocity of 1.5BV/h, collects eluent；
5) eluent crosses the hollow-fibre membrane that molecular cut off is 70,000, and permeate a and concentrate a is collected respectively；Will concentration
Liquid a crosses the hollow-fibre membrane that molecular cut off is 550,000, collects permeate b；Merge permeate a and permeate b；
6) medicinal extract that relative density is 1.15, freeze-drying are concentrated at 35 DEG C, you can.
Detected through HPLC, up to 99.9%, it is 96.1% to be computed recovery rate to flavones purity.
Embodiment 4
The method that flavones is extracted from pomelo peel, including following preparation process：
1) it is 35% to take pomelo peel and dry to aqueous component, is crushed to 90 mesh；
2) by the pomelo peel after crushing according to 1:14 weight is cut at a high speed than the ethanol solution for adding volumetric concentration to be 70%
Mulser treatment 28min is cut, rotating speed is 2000r/min；
3) the ultrasonic wave extraction 25min at a temperature of 65KHz frequencies and 40 DEG C, obtains flavones crude extract；
4) by flavones crude extract by macroporous adsorbent resin column chromatography, the volumetric concentration with 3 times of resin volume is 70%
Ethanol solution eluted for eluant, eluent, ethanol solution is eluted with the flow velocity of 1.2BV/h, collects eluent；
5) eluent crosses the hollow-fibre membrane that molecular cut off is 80,000, and permeate a and concentrate a is collected respectively；Will concentration
Liquid a crosses the hollow-fibre membrane that molecular cut off is 500,000, collects permeate b；Merge permeate a and permeate b；
6) medicinal extract that relative density is 1.18, freeze-drying are concentrated at 35 DEG C, you can.
Detected through HPLC, up to 99.6%, it is 96.1% to be computed recovery rate to flavones purity.
Embodiment 5
The method that flavones is extracted from pomelo peel, including following preparation process：
1) it is 40% to take pomelo peel and dry to aqueous component, is crushed to 80 mesh；
2) by the pomelo peel after crushing according to 1:16 weight is cut at a high speed than the ethanol solution for adding volumetric concentration to be 65%
Mulser treatment 30min is cut, rotating speed is 1800r/min；
3) the ultrasonic wave extraction 28min at a temperature of 85KHz frequencies and 35 DEG C, obtains flavones crude extract；
4) by flavones crude extract by macroporous adsorbent resin column chromatography, the volumetric concentration with 2 times of resin volume is 75%
Ethanol solution eluted for eluant, eluent, ethanol solution is eluted with the flow velocity of 0.8BV/h, collects eluent；
5) eluent crosses the hollow-fibre membrane that molecular cut off is 50,000, and permeate a and concentrate a is collected respectively；Will concentration
Liquid a crosses the hollow-fibre membrane that molecular cut off is 450,000, collects permeate b；Merge permeate a and permeate b；
6) medicinal extract that relative density is 1.2, freeze-drying are concentrated at 35 DEG C, you can.
Detected through HPLC, up to 99.8%, it is 95.4% to be computed recovery rate to flavones purity.
Claims (10)
1. the method that flavones is extracted from pomelo peel, it is characterised in that including following preparation process：
1) pomelo peel drying is taken, is crushed；
2) by the pomelo peel after crushing according to 1:8~16 weight ratio addition ethanol solution, high-speed shearing emulsion machine treatment 22~
30min, rotating speed is 1800~2800r/min；
3) 15~28min of ultrasonic wave extraction under 35~85KHz frequencies, obtains flavones crude extract；
4) flavones crude extract is eluted by macroporous adsorbent resin column chromatography by eluant, eluent of ethanol solution, is collected wash-out
Liquid；
5) eluent crosses the hollow-fibre membrane that molecular cut off is 5~80,000, and permeate a and concentrate a is collected respectively；Will concentration
Liquid a crosses the hollow-fibre membrane that molecular cut off is 45~600,000, collects permeate b；Merge permeate a and permeate b；
6) concentrate, dry, you can.
2. it is according to claim 1 from pomelo peel extract flavones method, it is characterised in that：The step 1) in, shaddock
It is 30~40% that sub- skin is dried to aqueous component.
3. it is according to claim 2 from pomelo peel extract flavones method, it is characterised in that：The step 1) in, powder
It is broken to 80~120 mesh.
4. it is according to claim 1 from pomelo peel extract flavones method, it is characterised in that：The step 2) in, second
The volumetric concentration of alcoholic solution is 65~75%.
5. it is according to claim 1 from pomelo peel extract flavones method, it is characterised in that：The step 3) in, surpass
Temperature when sound wave is extracted is 35~55 DEG C.
6. it is according to claim 1 from pomelo peel extract flavones method, it is characterised in that：The step 4) in, second
The addition of alcoholic solution is 2~6 times of resin volume.
7. it is according to claim 6 from pomelo peel extract flavones method, it is characterised in that：The step 4) in, second
The volumetric concentration of alcoholic solution is 55~75%.
8. it is according to claim 7 from pomelo peel extract flavones method, it is characterised in that：The step 4) in, second
Alcoholic solution is eluted with the flow velocity of 0.8~2.2BV/h.
9. it is according to claim 1 from pomelo peel extract flavones method, it is characterised in that：The step 6) in,
The medicinal extract that relative density is 1.1~1.2 is concentrated at 35 DEG C.
10. it is according to claim 9 from pomelo peel extract flavones method, it is characterised in that：The step 6) in, it is cold
It is lyophilized dry.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108383885A (en) * | 2018-05-02 | 2018-08-10 | 孙波 | From the technique and its purposes in anti-inflammatory for extracting Sophoricoside in the Fructus Sophorae |
| CN108514570A (en) * | 2018-04-26 | 2018-09-11 | 王洲 | The extraction process of Fructus Sophorae general flavone and its purposes in treating hyperlipidemia |
| CN113105513A (en) * | 2021-03-25 | 2021-07-13 | 华南农业大学 | Process for extracting flavone from shaddock peel |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104814987A (en) * | 2015-05-18 | 2015-08-05 | 天津工业大学 | Method for extracting total flavonoids from hibiscus manihot |
| CN105878487A (en) * | 2014-12-22 | 2016-08-24 | 南京海恒医药科技有限公司 | Application of pomelo peel in preparing nootropic drugs |
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2017
- 2017-03-29 CN CN201710195440.0A patent/CN106822315A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105878487A (en) * | 2014-12-22 | 2016-08-24 | 南京海恒医药科技有限公司 | Application of pomelo peel in preparing nootropic drugs |
| CN104814987A (en) * | 2015-05-18 | 2015-08-05 | 天津工业大学 | Method for extracting total flavonoids from hibiscus manihot |
Non-Patent Citations (1)
| Title |
|---|
| 滑聚娜等: "基于高剪切分散乳化技术的黄芪中黄酮类化合物提取方法及动力学研究", 《分析化学研究报告》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108514570A (en) * | 2018-04-26 | 2018-09-11 | 王洲 | The extraction process of Fructus Sophorae general flavone and its purposes in treating hyperlipidemia |
| CN108383885A (en) * | 2018-05-02 | 2018-08-10 | 孙波 | From the technique and its purposes in anti-inflammatory for extracting Sophoricoside in the Fructus Sophorae |
| CN108383885B (en) * | 2018-05-02 | 2021-07-23 | 孙波 | Process for extracting sophoricoside from fructus Sophorae and its application in anti-inflammation |
| CN113105513A (en) * | 2021-03-25 | 2021-07-13 | 华南农业大学 | Process for extracting flavone from shaddock peel |
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Application publication date: 20170613 |