CN106728037A - The extraction process of general flavone in a kind of tree peony seed peel - Google Patents
The extraction process of general flavone in a kind of tree peony seed peel Download PDFInfo
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- CN106728037A CN106728037A CN201611137405.5A CN201611137405A CN106728037A CN 106728037 A CN106728037 A CN 106728037A CN 201611137405 A CN201611137405 A CN 201611137405A CN 106728037 A CN106728037 A CN 106728037A
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- tree peony
- peony seed
- general flavone
- seed peel
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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)
- A61K36/71—Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
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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)
- A61K36/65—Paeoniaceae (Peony family), e.g. Chinese peony
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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 a kind of extraction process of general flavone in tree peony seed peel, belong to Chinese herbal medicine extractive technique field, comprise the following steps, 1)The pretreatment of macroreticular resin:By the macroreticular resin 60h of soaked in absolute ethyl alcohol 40, make it fully swelling, be fitted into chromatographic column, then use alcohol flushing chromatographic column, be washed till in eluate untill adding appropriate distilled water without white opacity, be then washed to without alcohol taste with distillation, leaching is standby;2)The extraction of general flavone:Tree peony seed peel extract solution is slow transitted through by step 1)The resin column of middle macroreticular resin composition, the solution remained in post is washed away with distilled water, then flows through resin column with the flow velocity of 0.20 0.40ml/s with eluent solution, collects eluent, is concentrated under reduced pressure into dry, obtains final product tree peony seed peel general flavone.The extraction process is easy to operate, and extraction effect is good.
Description
Technical field
The present invention relates to a kind of extraction process of general flavone in tree peony seed peel, belong to technical field of natural product extraction.
Background technology
Flavone compound is widely present in nature, belongs to plant produces during long-term natural selection some
Secondary metabolite.Flavone compound can be divided into more than 10 classification:Flavones, flavanols, isoflavones, flavanone, double hydrogen
Flavonols, lane, flavanones, anthocyanidin, chalcone, chromone etc., it has now been found that about more than 4000 plant flavone compound, mainly
It is present in leaf, fruit, root, the Pi Zhong of plant.Flavone compound has:Anti-oxidant, scavenging activated oxygen;Regulation cardiovascular system
System;Anticancer, protective effect on cancer risk;Anti-inflammatory, immune and anti-aging effects;Endocrine systemic effect;Bioflavonoid also has absorption
Ultraviolet radioactive, cough-relieving, eliminating the phlegm, rush down under, spasmolysis, improve memory, antiallergy, promoting blood circulation and removing blood stasis, cholagogic and liver protection etc..
The method for extraction and purification of flavone compound is a lot, and conventional extracting method has water extraction method, organic solvent to extract
Method, microwave extraction method, ultrasonic extraction, supercritical fluid extraction etc..The side of conventional separating and purifying flavone class compound
Method has silica gel column chromatography, Thin-layer chromatography, sephadex column chromatography, paper chromatography, TLC, lead salt to sink
Shallow lake, macroporous resin adsorption partition method etc..Wherein macroporous resin adsorption partition method is industrially used for preparing rich in flavonoid
Thing extract is most widely used.
Macroporous absorbent resin is the organic polymer adsorbent that the sixties in 20th century grows up.Macroporous absorbent resin is suction
The separation material that screening principle is combined is echoed, its adsorptivity is due to the result of Van der Waals force or generation hydrogen bond, screening
Principle is by itself cellular structure is determined.Organic compound according to absorption affinity difference and molecular weight size,
Eluted through certain solvent on macroporous absorbent resin and separated, this causes the purification of organic compound especially water soluble compound
Greatly simplified.Macroporous absorbent resin has the shadow that physical and chemical stability is high, adsorptive selectivity is strong, not existed by inorganic matter
Ring, regeneration is easy, desorption condition is gentle, usage cycles are long, the advantages of save expense, it is to avoid separated with Solvent Extract methods and
Difficult, loss that the organic solvent that causes is reclaimed is big, high cost, the shortcomings of inflammable and explosive, environmental pollution is serious.Macroporous absorbent resin
It is widely used in environmental protection, food, field of medicaments, macroporous absorbent resin is in Chinese herbal medicine effective ingredientses polishing purification
Application also increase year by year, separation in Chemical Constituents of Chinese Traditional And Folk Medicine, the application in enrichment are also increasingly valued by people.
The content of the invention
For the problem that above-mentioned prior art is present, the present invention provides a kind of extraction process of general flavone in tree peony seed peel,
Easy to operate, extraction effect is good.
To achieve these goals, the extraction process of general flavone, specifically includes in a kind of tree peony seed peel that the present invention is used
Following steps,
1)The pretreatment of macroreticular resin:By macroreticular resin soaked in absolute ethyl alcohol 40-60 h, make it fully swelling, load chromatography
In post, then alcohol flushing chromatographic column is used, be washed till in eluate untill adding appropriate distilled water without white opacity, then with distillation
It is washed to without alcohol taste, leaching is standby;
2)The extraction of general flavone:Tree peony seed peel extract solution is slow transitted through by step 1)The resin column of middle macroreticular resin composition, uses
Distilled water washes away the solution remained in post, then flows through resin column with the flow velocity of 0.20-0.40 ml/s with eluent solution, collects
Eluent, is concentrated under reduced pressure into dry, obtains final product tree peony seed peel general flavone.
As improvement, the step 1)The addition of distilled water is 4-6 times of eluate volume in eluate.
As improvement, the step 1)Any one or its mixing in middle use HZ802, HZ801 macroreticular resin.
As improvement, the step 2)The middle eluent solution for using is the ethanol solution of 50%-70% volumetric concentrations.
As a further improvement, the step 2)In, the ethanol solution that concentration is 60% is used with the flow velocity stream of 0.29mL/s
Cross resin column.
The preparation of tree peony seed peel extract solution can be obtained using conventional extractive technique and can such as use ultrasonic wave extraction in the present invention
Method, is extractant with 60% ethanol, by tree peony seed peel raw material and the feed liquid mass ratio 1 of extractant:20, filtered after extracting 1.5h
Obtain final product tree peony seed peel extract solution.
Compared with prior art, the present invention carries out adsorbing and extracting using HZ802, HZ801 series macroreticular resin, and the series is big
Macroporous adsorbent resin is that, with styrene and propionic ester as monomer, addition Ethenylbenzene is crosslinking agent, and toluene, dimethylbenzene are pore-foaming agent, it
The polymerization that is cross-linked with each other form porous skeleton structure.What macroporous absorbent resin was utilized is physical absorption principle, adsorptivity be by
In Van der Waals force or the result of generation hydrogen bond.In the preparation of peony seeds flavonoid material, macroporous absorbent resin has two
Particular advantages:One is, macroporous absorbent resin flow velocity is very fast, and production efficiency is high;Two are, macroporous absorbent resin is cheap, production
Low cost.Simple to operate, low cost of the invention, it is easy to industrialize, the general flavone content for obtaining is higher, separates flow velocity soon, separates
Efficiency high.
Specific embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, below by embodiment, the present invention is entered
Row is further described.However, it should be understood that the specific embodiments described herein are merely illustrative of the present invention, and without
In limitation the scope of the present invention.Unless otherwise defined, all of technical term used herein and scientific terminology with belong to this
The implication that the those skilled in the art of invention are generally understood that is identical, the art for being used in the description of the invention herein
Language is intended merely to describe the purpose of specific embodiment, it is not intended that in the limitation present invention.
Embodiment one
The extraction process of general flavone, specifically includes following steps in a kind of tree peony seed peel,
1)The pretreatment of macroreticular resin:Using HZ802 macroreticular resins, soaked in absolute ethyl alcohol 48h is used, make it fully swelling, loaded
In chromatographic column, then chromatographic column is rinsed with absolute ethyl alcohol, be washed till in eluate absolute ethyl alcohol and add appropriate distilled water (v/v, 1:5)
Untill without white opacity, then it is washed to without alcohol taste with distillation, leaching is standby;
2)The extraction of general flavone:The tree peony seed peel extract solution that concentration is 1.14 mg/mL is slow transitted through by step 1)Middle macropore tree
The resin bed of fat composition, removes in post the solution of residual with the washing of 1000mL, then with the ethanol solution that concentration is 60% with
The flow velocity of 0.29ml/s flows through resin column, collects eluent, is concentrated under reduced pressure into dry, obtains final product tree peony seed peel general flavone, and content is
70.4%。
Embodiment two
The extraction process of general flavone, specifically includes following steps in a kind of tree peony seed peel,
1)The pretreatment of macroreticular resin:Using HZ801 macroreticular resins, with the h of soaked in absolute ethyl alcohol 48, make it fully swelling, load
In chromatographic column, then alcohol flushing chromatographic column is used, be washed till in eluate and add appropriate distilled water (v/v, 1:5) it is without white opacity
Only, then it is washed to without alcohol taste with distillation, leaching is standby;
2)The extraction of general flavone:By concentration for 1.14 mg/mL tree peony seed peel extract solutions are slow transitted through by step 1)Middle macroreticular resin
The resin bed of composition, the solution for going to be remained in post with the washing of 1000mL, then with the ethanol solution that concentration is 60% with 0.29ml/s
Flow velocity flow through resin column, collect eluent, be concentrated under reduced pressure into dry, obtain final product tree peony seed peel general flavone, content is 69.8%.
Comparative example 1
The extraction process of general flavone, specifically includes following steps in a kind of tree peony seed peel,
1)The pretreatment of macroreticular resin:Using DA201 macroreticular resins, soaked in absolute ethyl alcohol 48h is used, make it fully swelling, loaded
In chromatographic column, then alcohol flushing chromatographic column is used, be washed till in eluate and add appropriate distilled water (v/v, 1:5) it is without white opacity
Only, then it is washed to without alcohol taste with distillation, leaching is standby;
2)The extraction of general flavone:By concentration for 1.14 mg/mL tree peony seed peel extract solutions are slow transitted through by step 1)Middle macroreticular resin
The resin bed of composition, with the washing of 1000mL go in post remain solution, then with the ethanol solution that volumetric concentration is 60% with
The flow velocity of 0.15ml/s flows through resin column, collects eluent, is concentrated under reduced pressure into dry, obtains final product tree peony seed peel general flavone, and content is
59.4%。
Comparative example 2
The extraction process of general flavone, specifically includes following steps in a kind of tree peony seed peel,
1)The pretreatment of macroreticular resin:Using AB-8 macroreticular resins, soaked in absolute ethyl alcohol 48h is used, make it fully swelling, load layer
In analysis post, then alcohol flushing chromatographic column is used, be washed till in eluate and add appropriate distilled water (v/v, 1:5) it is without white opacity
Only, then it is washed to without alcohol taste with distillation, leaching is standby;
2)The extraction of general flavone:By concentration for 1.14 mg/mL tree peony seed peel extract solutions are slow transitted through by step 1)Middle macroreticular resin
The resin bed of composition, with the washing of 1000mL go in post remain solution, then with the ethanol solution that volumetric concentration is 60% with
The flow velocity of 0.15ml/s flows through resin column, collects eluent, is concentrated under reduced pressure into dry, obtains final product tree peony seed peel general flavone, and content is
60.3%。
Meanwhile, compared with the existing conventional extraction process by polycaprolactam, the present invention is carried out using macroreticular resin
Absorption, compared with polycaprolactam technique, macroporous absorbent resin is, with styrene and propionic ester as monomer, to add Ethenylbenzene to hand over
Connection agent, toluene, dimethylbenzene are pore-foaming agent, and their polymerizations that are cross-linked with each other form porous skeleton structure.And polyamide is gathered by acid amides
The family macromolecule material for closing, is called nylon, polyamide fibre.Secondly, principle is different.What macroporous absorbent resin was utilized is that physics is inhaled
Attached principle, adsorptivity is due to the result of Van der Waals force or generation hydrogen bond.The principle of polyamide column is mainly hydrogen bond and double layers
Two kinds of analysis.
In the preparation of peony seeds flavonoid material, macroporous absorbent resin has two particular advantages:One is, macropore is inhaled
Attached resin flow velocity is very fast, and production efficiency is high;Two are, macroporous absorbent resin is cheap, low production cost.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, it is all in essence of the invention
Any modification, equivalent or improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (5)
1. in a kind of tree peony seed peel general flavone extraction process, it is characterised in that specifically include following steps:
1)The pretreatment of macroreticular resin:By macroreticular resin soaked in absolute ethyl alcohol 40-60h, make it fully swelling, load chromatographic column
In, then alcohol flushing chromatographic column is used, it is washed till in eluate untill adding appropriate distilled water without white opacity, then use distilled water
It is washed till without alcohol taste, leaching is standby;
2)The extraction of general flavone:Tree peony seed peel extract solution is slow transitted through by step 1)The resin column of middle macroreticular resin composition, uses
Distilled water washes away the solution remained in post, then flows through resin column with the flow velocity of 0.20-0.40ml/s with eluent solution, and collection is washed
De- liquid, is concentrated under reduced pressure into dry, obtains final product tree peony seed peel general flavone.
2. in a kind of tree peony seed peel as claimed in claim 1 general flavone extraction process, it is characterised in that the step 1)Wash
The addition for going out distilled water in liquid is 4-6 times of eluate volume.
3. in a kind of tree peony seed peel as claimed in claim 1 general flavone extraction process, it is characterised in that the step 1)In
Using any one or its mixing in HZ802, HZ801 macroreticular resin.
4. in a kind of tree peony seed peel as claimed in claim 3 general flavone extraction process, it is characterised in that the step 2)In
The eluent solution for using is the ethanol solution of 50%-70% concentration.
5. in a kind of tree peony seed peel as claimed in claim 4 general flavone extraction process, it is characterised in that the step 2)
In, use the ethanol solution that concentration is 60% to flow through resin column with the flow velocity of 0.29mL/s.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103766913A (en) * | 2014-01-10 | 2014-05-07 | 河南科技大学 | Method for extracting total stilbene compound from penoy seeds |
CN104435134A (en) * | 2014-11-13 | 2015-03-25 | 中国科学院山西煤炭化学研究所 | Method for extracting flavonoids from peony seed hulls |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103766913A (en) * | 2014-01-10 | 2014-05-07 | 河南科技大学 | Method for extracting total stilbene compound from penoy seeds |
CN104435134A (en) * | 2014-11-13 | 2015-03-25 | 中国科学院山西煤炭化学研究所 | Method for extracting flavonoids from peony seed hulls |
Non-Patent Citations (1)
Title |
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程雪芬等: "牡丹籽皮中总黄酮提取工艺探究", 《现代食品》 * |
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Application publication date: 20170531 |