CN109260271A - A method of simulating mobile chromatogram purification duck wheat shell flavones - Google Patents
A method of simulating mobile chromatogram purification duck wheat shell flavones Download PDFInfo
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- CN109260271A CN109260271A CN201811420403.6A CN201811420403A CN109260271A CN 109260271 A CN109260271 A CN 109260271A CN 201811420403 A CN201811420403 A CN 201811420403A CN 109260271 A CN109260271 A CN 109260271A
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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Abstract
The present invention relates to a kind of methods for simulating mobile chromatogram purification duck wheat shell flavones, and this method is using duck wheat shell flavone extractive as raw material, after pretreatment, duck wheat shell flavone extractive concentration is allocated as 20 mg/mL-30 mg/mL；Simulate the mobile pretreated duck wheat shell flavone extractive of chromatogram purification, mobile chromatographic equipment is simulated to be made of 20 root chromatogram columns, it is divided into adsorption zone, refining zone, desorption zone, renewing zone, water wash zone, pass through rotary valve control charging, discharging, the chromatographic column quantity in five areas is respectively 6,3,5,3,3, is connected in series between each area；Each area works at the same time, and after reaching switching time, every root chromatogram column moves a column position clockwise, and successively continuous operation is realized in operation in this manner；The obtained flavones of duck wheat shell after purification continues to be concentrated in vacuo, freeze-drying, obtains purification duck wheat shell flavones.The present invention can continuous production, reduce production loss.
Description
One, technical field:
The present invention relates to mobile chromatographic separation and purification technology is simulated in field of food industry, and in particular to be a kind of simulation
The method of mobile chromatogram purification duck wheat shell flavones.
Two, background technique:
Tartary buckwheat (tartary buckwheat) also known as triangle wheat, also referred to as hull buckwheat, are to collect nutrition in the world today, are protected
Strong, in one of the natural health care of one, duck wheat shell is the by-product of tartary buckwheat production for medical treatment, about buckwheat total amount
24.4%, is currently, duck wheat shell is largely simply discarded, and only small part is used as pillow filler material, or directly
Burning, results in waste of resources.Research shows that buckwheat shell has anti-oxidant, hypoglycemic, blood lipid, sterilization is antibacterial and other effects, and plays
The substance of these pharmacological activity is mainly flavone compound contained in buckwheat.Therefore, duck wheat shell extracting flavonoids purify
The research of method is more, common method have hot water extraction method, supercritical ultrasonics technology, surfactant-ultrasonic synergistic extraction method,
Supercritical CO2The methods of extraction, macroporous resin column chromatography method, high speed adverse current chromatogram.But existing method is there are at high cost,
The problems such as low efficiency, purity is unstable, complicated for operation, not can be carried out industrialization production.
Chinese invention patent application 201210055553.8 discloses a kind of subcritical abstraction tartary buckwheat Flavone
No purification step is only simply extracted in method, the patent application, and the purity of gained flavones is lower；Chinese invention patent application
201210136437.9 disclosing a kind of water-soluble tartary buckwheat general flavone extract and preparation method thereof, which uses water
Extraction, alcohol extracting, drying and other steps purify water-soluble tartary buckwheat general flavone, and the complex process time is longer；Chinese invention patent Shen
201510271179.9 a kind of preparation method of tartary buckwheat bran general flavone please be disclosed, the patent application supercritical CO2Extraction,
Large pore resin absorption column purifying has obtained higher purity and yield, but this method is using single column chromatographic, is intermittent
Operating procedure, solvent consumption is big, resin utilization rate is low, production efficiency is low, has been not suitable for the needs of existing market competition, is badly in need of
Efficient industrialization duck wheat shell flavones purification technique.
Simulated Moving Bed Chromatography (SMB) purification technique is a kind of efficient means of purification, and relative to single column chromatographic, SMB is pure
The resin utilization rate of change technology is high, and inlet amount is big, eluting agent is small, can be continuously produced, production efficiency is higher.Currently, not
See the report of Simulated Moving Bed Chromatography (SMB) purifying duck wheat shell flavones technical research.
Three, summary of the invention:
The object of the present invention is to provide a kind of method for simulating mobile chromatogram purification duck wheat shell flavones, the mobile chromatographies of this simulation
The method of purifying duck wheat shell flavones is used to solve in the prior art can not efficient, serialization purifying duck wheat shell flavones difficulty
Topic.
The technical solution adopted by the present invention to solve the technical problems is: the mobile chromatogram purification duck wheat shell of this simulation is yellow
The method of ketone:
Using duck wheat shell flavone extractive as raw material, after concentrated, filtering pretreatment, by duck wheat shell flavone extractive concentration tune
With for 20 mg/mL-30 mg/mL, and it is delivered to the mobile chromatography of simulation；
Using the mobile pretreated duck wheat shell flavone extractive of chromatogram purification is simulated, mobile chromatographic equipment is simulated by 20 colors
Compose column composition, 20 root chromatogram columns are separately mounted on rotary valve, rotary valve be arranged on the rotating shaft, by rotary valve control into
Material, discharging；It simulates mobile chromatography and is divided into adsorption zone, refining zone, desorption zone, renewing zone, the region of water wash zone five, five areas
Chromatographic column quantity be respectively 6,3,5,3,3, be all made of concatenated connection type between each area；Each area all has
Feed inlet 1, discharge port 1, adsorption zone, refining zone, desorption zone, renewing zone feed inlet be each area along clockwise direction
First root chromatogram column, the feed inlet of water wash zone are last root chromatogram column of the area along clockwise direction；It is each in the process of running
Area works at the same time, when running between reach switching time after, every root chromatogram column clockwise move a column position, in this manner according to
Continuous operation is realized in secondary operation；
Adsorption zone, refining zone, desorption zone, renewing zone, water wash zone feeding liquid be respectively pre-process after duck wheat shell extracting flavonoids
Liquid, 15%-25% ethanol water, 55%-65% ethanol water, 90%-100% ethanol water, deionized water；Switching time is
1000-1500s；
The obtained flavones of duck wheat shell after purification continues to be concentrated in vacuo, and 30 DEG C -50 DEG C of thickening temperature, is freezed after concentration
It is dry, obtain purification duck wheat shell flavones.
SMB chromatographic column fixed phase is AB-8 or X-5 low pole macroreticular resin or non-polar macroporous resin in above scheme.
Adsorption zone in above scheme, refining zone, desorption zone, renewing zone, water wash zone flow velocity be respectively 1-3BV/h, 5-
8BV/h,5-10BV/h,5-10BV/h,5-12BV/h；Operating temperature is 20 DEG C -30 DEG C；Purify obtained duck wheat shell flavones
Purity is 80%~90%, yield is 80~90%.
The utility model has the advantages that
Present invention process operating cost is low, and input concentration is high, the product purity (80%~90%) that purifies, yield (80~
90%) higher, it saves ethanol consumption 80%-120%, reduce water consumption 150%-200%, reduce subsequent concentration cost, simplify operation
Step, 20 root chromatogram column of equipment, increase resin utilization rate, reduce production loss, can continuous production, improving production efficiency.
Four, Detailed description of the invention:
Fig. 1 is the process flow chart that the present invention simulates mobile chromatogram purification duck wheat shell flavones.
In figure: 1 chromatographic column, 2 desorption flow containers, 3 purification flow containers, 4 absorption flow containers, 5 washing flow containers, 6 regeneration flow containers,
7 waste liquid tanks, 8 purifying tanks, 9 controllers, 10 thermostats.
Five, specific embodiment:
Following further describes the present invention with reference to the drawings:
As shown in Figure 1, the present invention using the method for simulating mobile chromatogram purification duck wheat shell flavones, simulate mobile chromatographic equipment by
20 root chromatogram columns 1 composition, 1 internal diameter of chromatographic column, 25 mm, 1000 mm of length, the rounded distribution of 20 root chromatogram column 1,20 root chromatogram columns
1 is separately mounted on rotary valve, and rotary valve is arranged on the rotating shaft, passes through rotary valve control charging, discharging；Simulate mobile chromatography
It is divided into adsorption zone, refining zone, desorption zone, renewing zone, the region of water wash zone five, adsorption zone chromatographic column quantity is 6, refining zone color
Composing column quantity is 3, and desorption zone chromatographic column quantity is 5, and renewing zone chromatographic column quantity is 3, and water wash zone chromatographic column quantity is 3
Root is all made of concatenated connection type between each area；Each area all has feed inlet 1, discharge port 1, adsorption zone, refining zone,
Desorption zone, renewing zone feed inlet be the first root chromatogram column of each area along clockwise direction, the feed inlet of water wash zone is the area
Last root chromatogram column along clockwise direction；Each area works at the same time in the process of running, when running between reach switching time
Afterwards, every root chromatogram column moves a column position clockwise, and successively continuous operation is realized in operation in this manner.Mobile chromatography is simulated to set
It is equipped with controller 9, thermostat 10, adsorption zone is provided with absorption flow container 4, and adsorption liquid is that concentration is 20 mg/mL-30 after pre-processing
Mg/mL duck wheat shell flavone extractive；Refining zone is provided with purification flow container 3, and refined liquid is that mass percent concentration is 15%-25%
Ethyl alcohol；Desorption zone is provided with desorption flow container 2, and stripping liquid is the ethyl alcohol that mass percent concentration is 35%-45%；Renewing zone setting
There is regeneration flow container 6, regenerated liquid is the ethyl alcohol that mass percent concentration is 80%-100%, and the concentration of acetic acid is quality in the present invention
Percent concentration；Water wash zone setting washing flow container 5, water lotion is deionized water；Waste liquid is all flowed into waste liquid tank 7, after purification
Duck wheat shell flavones be collected into purifying tank 8 in.
Embodiment 1:
This method for simulating mobile chromatogram purification duck wheat shell flavones:
Using duck wheat shell flavone extractive as raw material, after concentrated, filtering pretreatment, by duck wheat shell flavone extractive concentration tune
With for 200 mg/mL, and it is delivered to the mobile chromatography of simulation.
Simulate mobile chromatogram purification duck wheat shell flavones: by duck wheat shell flavone extractive obtained above through the simulation
Mobile chromatography is purified, and the mobile chromatography of the simulation includes 20 root chromatogram columns, is divided into adsorption zone, refining zone, desorption zone, regeneration
Area and water wash zone, the chromatographic column quantity in five areas are respectively 6,3,5,3,3.Concatenated company is all made of between each area
Connect mode, all have feed inlet 1, discharge port 1, adsorption zone, refining zone, desorption zone, renewing zone feed inlet be the area
First root chromatogram column (clockwise direction), only water wash zone feed inlet are last root chromatogram column (clockwise direction) in the area；
Each area works at the same time in the process of running, when running between reach switching time after, every root chromatogram column clockwise move a column
Position, successively continuous operation is realized in operation in this manner；The feeding liquid of adsorption zone is that concentration is 25mg/mL tartary buckwheat after pre-processing
Shell flavone extractive, refining zone feeding liquid be 20% ethanol water, desorption zone feeding liquid be 60% ethanol water, regeneration
The feeding liquid in area is that the feeding liquid of 95% ethanol water and water wash zone is deionized water；The flow velocity of adsorption zone is 1.7BV/h, essence
The flow velocity in area processed is 5.2BV/h, the flow velocity of desorption zone is 5.6BV/h, the flow velocity of renewing zone is 5.6BV/h, the flow velocity of water wash zone
For 7.0BV/h；Switching time is 1260 s；SMB chromatographic column fixed phase is AB-8 macroreticular resin；Operating temperature is 25 DEG C.
After duck wheat shell flavones is concentrated in vacuo after purification, 45 DEG C of thickening temperature, frozen dried is carried out after concentration, i.e.,
Duck wheat shell flavones must be refined.
The duck wheat shell flavones purity 88.2% that the present embodiment purifies, yield 80.6%.
Embodiment 2:
This method for simulating mobile chromatogram purification duck wheat shell flavones:
Using duck wheat shell flavone extractive as raw material, after concentrated, filtering pretreatment, by duck wheat shell flavone extractive concentration tune
With for 20 mg/mL, and it is delivered to the mobile chromatography of simulation.
Simulate mobile chromatogram purification duck wheat shell flavones: by duck wheat shell flavone extractive obtained above through the simulation
Mobile chromatography is purified, and it is same as Example 1 to simulate mobile chromatography, wherein adsorption zone, refining zone, desorption zone, renewing zone and
The feeding liquid of water wash zone is respectively 20 mg/mL of duck wheat shell flavone extractive, 15% ethanol water, 65% ethyl alcohol after pre-processing
Aqueous solution, 100% ethanol water and deionized water；Adsorption zone, refining zone, desorption zone, renewing zone and the flow velocity of water wash zone difference
For 1.7BV/h, 5.2BV/h, 5.6BV/h, 6.4BV/h, 8.1BV/h；Switching time is 1080s；SMB chromatographic column fixed phase is X-
5 macroreticular resins；Operating temperature is 30 DEG C.
After duck wheat shell flavones is concentrated in vacuo after purification, 50 DEG C of thickening temperature, after concentration carry out frozen dried to get
Refine duck wheat shell flavones.
The duck wheat shell flavones purity 84.6% that the present embodiment purifies, yield 84.9%.
Embodiment 3:
This method for simulating mobile chromatogram purification duck wheat shell flavones:
Using duck wheat shell flavone extractive as raw material, after concentrated, filtering pretreatment, by duck wheat shell flavone extractive concentration tune
With for 30 mg/mL, and it is delivered to the mobile chromatography of simulation.
Simulate mobile chromatogram purification duck wheat shell flavones: by duck wheat shell flavone extractive obtained above through the simulation
Mobile chromatography is purified, and it is same as Example 1 to simulate mobile chromatography, wherein adsorption zone, refining zone, desorption zone, renewing zone and
The feeding liquid of water wash zone is respectively 30 mg/mL of duck wheat shell flavone extractive, 20% ethanol water, 60% ethyl alcohol after pre-processing
Aqueous solution, 90% ethanol water and deionized water；Adsorption zone, refining zone, desorption zone, renewing zone and the flow velocity of water wash zone difference
For 2.5BV/h, 6.3BV/h, 8.2BV/h, 8.8BV/h, 10.1BV/h；Switching time is 1080 s；SMB chromatographic column fixed phase is
AB-8 macroreticular resin；Operating temperature is 25 DEG C.
After duck wheat shell flavones is concentrated in vacuo after purification, 35 DEG C of thickening temperature, after concentration carry out frozen dried to get
Refine duck wheat shell flavones.
The duck wheat shell flavones purity 86.1% that the present embodiment purifies, yield 82.7%.
Embodiment 4:
This method for simulating mobile chromatogram purification duck wheat shell flavones:
Using duck wheat shell flavone extractive as raw material, after concentrated, filtering pretreatment, by duck wheat shell flavone extractive concentration tune
With for 25 mg/mL, and it is delivered to the mobile chromatography of simulation.
Simulate mobile chromatogram purification duck wheat shell flavones: by duck wheat shell flavone extractive obtained above through the simulation
Mobile chromatography is purified, and it is same as Example 1 to simulate mobile chromatography, wherein adsorption zone, refining zone, desorption zone, renewing zone and
The feeding liquid of water wash zone is respectively 25 mg/mL of duck wheat shell flavone extractive, 15% ethanol water, 65% ethyl alcohol after pre-processing
Aqueous solution, 100% ethanol water and deionized water；Adsorption zone, refining zone, desorption zone, renewing zone and the flow velocity of water wash zone difference
For 2.5BV/h, 5.9BV/h, 7.6BV/h, 7.8BV/h, 10.5BV/h；Switching time is 840s；SMB chromatographic column fixed phase is X-
5 macroreticular resins；Operating temperature is 30 DEG C.
After duck wheat shell flavones is concentrated in vacuo after purification, 45 DEG C of thickening temperature, after concentration carry out frozen dried to get
Refine duck wheat shell flavones.
The duck wheat shell flavones purity 83.7% that the present embodiment purifies, yield 87.2%.
Core of the invention technology is to simulate the technology of mobile chromatogram purification duck wheat shell flavones, obtains purity and yield is equal
Higher duck wheat shell flavones, this technique not only ensure that duck wheat shell flavones high-purity and high yield, also reside in entire technique
The saving of cost, process is easy, can be continuously produced etc. and to have distinct characteristic.
Claims (3)
1. a kind of method for simulating mobile chromatogram purification duck wheat shell flavones, it is characterised in that: the mobile chromatogram purification of this simulation
The method of duck wheat shell flavones:
Using duck wheat shell flavone extractive as raw material, after concentrated, filtering pretreatment, by duck wheat shell flavone extractive concentration tune
With for 20 mg/mL-30 mg/mL, and it is delivered to the mobile chromatography of simulation；
Using the mobile pretreated duck wheat shell flavone extractive of chromatogram purification is simulated, mobile chromatographic equipment is simulated by 20 colors
Compose column composition, 20 root chromatogram columns are separately mounted on rotary valve, rotary valve be arranged on the rotating shaft, by rotary valve control into
Material, discharging；It simulates mobile chromatography and is divided into adsorption zone, refining zone, desorption zone, renewing zone, the region of water wash zone five, five areas
Chromatographic column quantity be respectively 6,3,5,3,3, be all made of concatenated connection type between each area；Each area all has
Feed inlet 1, discharge port 1, adsorption zone, refining zone, desorption zone, renewing zone feed inlet be each area along clockwise direction
First root chromatogram column, the feed inlet of water wash zone are last root chromatogram column of the area along clockwise direction；It is each in the process of running
Area works at the same time, when running between reach switching time after, every root chromatogram column clockwise move a column position, in this manner according to
Continuous operation is realized in secondary operation；
Adsorption zone, refining zone, desorption zone, renewing zone, water wash zone feeding liquid be respectively pre-process after duck wheat shell extracting flavonoids
Liquid, 15%-25% ethanol water, 55%-65% ethanol water, 90%-100% ethanol water, deionized water；Switching time is
1000-1500s；
The obtained flavones of duck wheat shell after purification continues to be concentrated in vacuo, and 30 DEG C -50 DEG C of thickening temperature, is freezed after concentration
It is dry, obtain purification duck wheat shell flavones.
2. the method according to claim 1 for simulating mobile chromatogram purification duck wheat shell flavones, it is characterised in that: described
SMB chromatographic column fixed phase is AB-8 or X-5 low pole macroreticular resin or non-polar macroporous resin.
3. the method according to claim 2 for simulating mobile chromatogram purification duck wheat shell flavones, it is characterised in that: described
Adsorption zone, refining zone, desorption zone, renewing zone, water wash zone flow velocity be respectively 1-3BV/h, 5-8BV/h, 5-10BV/h, 5-
10BV/h,5-12BV/h；Operating temperature is 20 DEG C -30 DEG C；Obtained duck wheat shell flavones purity is purified to be 80%~90%, receive
Rate is 80~90%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110152353A (en) * | 2019-06-18 | 2019-08-23 | 大连博迈科技发展有限公司 | A kind of continuous chromatography device and arasaponin production method |
| CN110656083A (en) * | 2019-08-30 | 2020-01-07 | 吉林农业大学 | Pre-adipocyte brown induction kit |
-
2018
- 2018-11-26 CN CN201811420403.6A patent/CN109260271B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| 周一鸣: "苦荞麸皮中黄酮类化合物的提取、分离及其抗氧化活性的研究", 《中国优秀硕士学位论文全文数据库•工程科技I辑》 * |
| 李朝阳等: ""模拟移动色谱在天然产物活性成分提取领域的研究进展"", 《科技信息》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110152353A (en) * | 2019-06-18 | 2019-08-23 | 大连博迈科技发展有限公司 | A kind of continuous chromatography device and arasaponin production method |
| CN110152353B (en) * | 2019-06-18 | 2024-05-28 | 大连博迈科技发展有限公司 | Continuous chromatographic device and production method of total saponins of panax notoginseng |
| CN110656083A (en) * | 2019-08-30 | 2020-01-07 | 吉林农业大学 | Pre-adipocyte brown induction kit |
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