CN109395427A - A kind of environment-friendly type glabridin extraction element and its technique - Google Patents
A kind of environment-friendly type glabridin extraction element and its technique Download PDFInfo
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- CN109395427A CN109395427A CN201910003005.2A CN201910003005A CN109395427A CN 109395427 A CN109395427 A CN 109395427A CN 201910003005 A CN201910003005 A CN 201910003005A CN 109395427 A CN109395427 A CN 109395427A
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- glabridin
- ethyl alcohol
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- ethanol solution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0088—Cascade evaporators
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/02—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in boilers or stills
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/04—Ortho-condensed systems
Abstract
The invention discloses a kind of environment-friendly type glabridin extraction element and its techniques, including ethyl alcohol configuration device, multiple glass chromatography columns are connected in ethyl alcohol configuration device side by side, each glass chromatography column is connected separately with the first chromatography liquid bath through the first isocon, second chromatography liquid bath and third chromatograph liquid bath, first chromatography liquid bath, the first chromatographic solution concentration kettle is connected separately on the outside of second chromatography liquid bath and third chromatography liquid bath, second chromatographic solution concentration kettle and third chromatographic solution concentration kettle, wherein the first chromatographic solution concentration kettle and the second chromatographic solution concentration kettle side are connected with alcohol recovering device, the other side is connected with the first rotary evaporator；The third chromatographic solution concentration kettle side connects alcohol recovering device, and the third chromatographic solution concentration kettle other side is connected with enrichment facility, and first rotary evaporator connects alcohol recovering device through the first return pipe.The present invention has the characteristics that DNA purity is various, production cost is low and energy conservation and environmental protection.
Description
Technical field
The present invention relates to a kind of glabridin extraction element and its technique, especially a kind of environment-friendly type glabridin extracts dress
It sets and its technique.
Background technique
Glabridin is one of the Main Flavonoids constituents in glycyrrhiza glabra, and glabridin can be in cytochromes due to it
Very strong free radical resisting oxidation is shown in oxidative system, can obviously inhibit in internal metabolic processes caused by from
By base, to have good inhibition melanogen, anti-inflammatory, anti-oxidant and antibacterial action, it is widely used in drug and makeup
Product field, market demand are larger.But glabridin extraction element on the market can only generally extract a kind of light of purity at present
Licoricidin powder, and the purity of glabridin after extraction fills between 10%-40% so that producer be needed to extract by multiple tracks
Set the glabridin powder product that can just obtain different purity, and by other devices to low-purity glabridin powder product into
Row secondary operation can just obtain the glabridin powder product of high-purity；To reduce extraction efficiency and the increasing to glabridin
Production cost and the energy consumption of relevant device are added.It gives up in addition, glabridin also needs to consume during the extraction process a large amount of processing
Material, and these waste materials can not be recycled by conventional extraction element mostly, to further improve glabridin
The waste of extraction cost and resource.So existing glabridin extraction element there are DNA purities single, high production cost and
The larger problem of raw material energy consumption.
Summary of the invention
The object of the present invention is to provide a kind of environment-friendly type glabridin extraction element and its techniques.It has extraction pure
The characteristics of degree is various, production cost is low and energy conservation and environmental protection.
Technical solution of the present invention: a kind of environment-friendly type glabridin extraction element, including ethyl alcohol configuration device, ethyl alcohol configuration
Multiple glass chromatography columns are connected on device side by side, each glass chromatography column is connected separately with the first chromatographic solution through the first isocon
Slot, the second chromatography liquid bath and third chromatograph liquid bath, and the first chromatography liquid bath, the second chromatography liquid bath and third chromatograph on the outside of liquid bath respectively
It is connected with the first chromatographic solution concentration kettle, the second chromatographic solution concentration kettle and third chromatographic solution concentration kettle, wherein the first chromatographic solution is concentrated
Kettle and the second chromatographic solution concentration kettle side are connected with alcohol recovering device, and the other side is connected with the first rotary evaporator；Described
Three chromatographic solution concentration kettle sides connect alcohol recovering device, and the third chromatographic solution concentration kettle other side is connected with enrichment facility, described
First rotary evaporator connects alcohol recovering device through the first return pipe.
In a kind of environment-friendly type glabridin extraction element above-mentioned, the ethyl alcohol configuration device includes that ethanol solution is prepared
Slot, ethanol solution make-up tank outside are connected separately with the first ethanol solution transfer tank and the second ethanol solution transfer tank, the first second
Alcoholic solution transfer tank and the second ethanol solution transfer tank are separately connected multiple glass chromatography columns through the second isocon.
In a kind of environment-friendly type glabridin extraction element above-mentioned, second isocon includes being connected to multiple glass
Multiple branch pipes on glass chromatographic column are connected with each other between every two branch pipe through connecting tube, are connected separately with first on the outside of connecting tube
Delivery pipe and the second delivery pipe, the first conveying tube end connect the first ethanol solution transfer tank, the second conveying tube end connection the
Diethyl alcoholic solution transfer tank.
In a kind of environment-friendly type glabridin extraction element above-mentioned, the alcohol recovering device includes three arranged side by side
Ethyl alcohol recycles condenser, and three ethyl alcohol recycling condenser sides are separately connected the first chromatographic solution concentration kettle, the concentration of the second chromatographic solution
Kettle and third chromatographic solution concentration kettle, three ethyl alcohol recycling condenser other sides are respectively connected with ethyl alcohol accumulator tank and ethyl alcohol recycling tail is solidifying
Device, ethyl alcohol recycle tail condenser side and connect ethyl alcohol accumulator tank, connects ethyl alcohol through third return pipe on the outside of ethyl alcohol accumulator tank and configure dress
It sets.
In a kind of environment-friendly type glabridin extraction element above-mentioned, the enrichment facility includes secondary concentration kettle, secondary dense
Contracting kettle side connects third chromatographic solution concentration kettle, and the secondary concentration kettle other side is connected separately with toluene metal bucket, purifying reflux condensation mode
Device and glabridin centrifuge, are connected with the second rotary evaporator on the outside of glabridin centrifuge, and the second rotary evaporator is through the
Two return pipes connect alcohol recovering device.
With a kind of glabridin extraction process of aforementioned extraction element, comprising the following steps:
1. preparing the ethanol water of 50% concentration in ethanol solution make-up tank, then it is respectively fed to through the second isocon
It is spare in first ethanol solution transfer tank and the second ethanol solution transfer tank, obtain A ethanol solution；
2. the crude flavonoid powder after weighing is respectively put into multiple glass chromatography columns, and it is mixed that polystyrene resin or silica gel is added
It closes uniformly, then removes insoluble impurity, obtain B flavones ethanol solution；
3. B flavones ethanol solution is separated by the polystyrene resin or silica gel being mixed in B flavones ethanol solution,
The glabridin ethyl alcohol water mixed liquid of different purity is obtained, C mixed liquor is obtained；
4. the C mixed liquor in multiple glass chromatography columns is respectively fed to the first chromatography liquid bath, by the content of glabridin
In two chromatography liquid baths and third chromatography liquid bath, wherein 20% glabridin content C mixed liquor below is sent into the first chromatography liquid bath,
The C mixed liquor of 20~40% glabridin contents is sent into the second chromatography liquid bath, and C mixed liquor more than 40% glabridin content is sent
Enter third chromatography liquid bath, successively obtains D mixed liquor, E mixed liquor and F mixed liquor；
5. D mixed liquor is sent into the first chromatographic solution concentration kettle and carries out concentration distillation, then vinasse is sent into the first rotation
Turn evaporator for decompression to be evaporated, obtains 20% concentration glabridin powder product below；E mixed liquor is sent into the second chromatographic solution
Concentration distillation is carried out in concentration kettle and obtains f1 concentrate, then dehydrated alcohol dissolved dilution is added into f1 concentrate, after filtering
It is sent into evaporated under reduced pressure in the first rotary evaporator to f2 concentrate, then by f2 concentrate, obtains the light Radix Glycyrrhizae of 20~40% concentration
Determine powder product；F mixed liquor is sent into third chromatographic solution concentration kettle be concentrated distilling and obtains f3 concentrate, then f3 is concentrated
Liquid is sent into enrichment facility and carries out secondary concentration, obtains the glabridin powder product of 90% concentration.
In a kind of glabridin extraction process above-mentioned, the enrichment facility is specific to the secondary concentration mode of f3 concentrate
Are as follows: f3 concentrate, acetone and toluene are sent into secondary concentration kettle by the mass ratio of 10:5:4 first, keep f3 dense by steam heating
Contracting liquid, which is dissolved in acetone toluene Mixed Solvent, obtains mixed liquor, and insulated and stirred cools after half an hour, makes in mixed liquor
Glabridin recrystallizes to form solid, then the solid is sent into glabridin centrifuge and is centrifugally separating to obtain filter cake, finally
Filter cake is sent into the second rotary evaporator evaporated under reduced pressure, obtains the glabridin powder product of 90% concentration.
Compared with prior art, the present invention passes through glass chromatography column, multiple chromatography liquid baths, multiple chromatographic solution concentration kettles and rotation
Turn the cooperation of evaporator, can the flavones ethanol solution of multiple groups various concentration is concentrated and be extracted simultaneously, so as to one
Secondary property obtains the glabridin powder product of different purity, reduces production cost of the invention and with DNA purity multiplicity
Feature；By the interconnection of enrichment facility and above-mentioned apparatus, it can also be purified during the extraction process, to obtain
The glabridin powder of high concentration further improves extraction diversity and finished product purity to glabridin；The present invention goes back root
Corresponding device quantity and connection type are optimized according to required finished product purity, making device during the extraction process can have well
Extraction stability and extraction efficiency, further reduced production cost of the invention and facilitate the control of producer；Pass through ethyl alcohol
The cooperation of configuration device, alcohol recovering device, the first rotary evaporator and the second rotary evaporator, can also be in glabridin
The alcohol gas generated when in purification process by evaporation carries out recycling and cooling liquid, and is delivered to ethanol solution make-up tank again
Middle secondary use, to further reduced production cost of the invention and there is energy-saving and environment-friendly effect.
In addition, cooperation of the present invention by multiple glass chromatography columns and the first isocon, can be further improved sweet to light
The fixed extraction efficiency of grass；By the cooperation of ethanol solution make-up tank, ethanol solution transfer tank and the second isocon, can effectively mention
Height is to the transfer efficiency of ethanol solution, to guarantee the extraction stability of glabridin.So the present invention has DNA purity more
The characteristics of sample, production cost be low and energy conservation and environmental protection.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention.
The label in accompanying drawing is: 1- ethyl alcohol configuration device, 2- the first chromatographic solution concentration kettle, 3- glass chromatography column, 4- first
Isocon, 5- first chromatograph liquid bath, and 6- second chromatographs liquid bath, and 7- third chromatographs liquid bath, 8- the second chromatographic solution concentration kettle, 9- ethyl alcohol
Recyclable device, the first rotary evaporator of 10-, 11- third chromatographic solution concentration kettle, 12- enrichment facility, the first return pipe of 13-, 101-
Ethanol solution make-up tank, 102- the first ethanol solution transfer tank, 103- the second ethanol solution transfer tank, the second isocon of 104-,
1041- branch pipe, 1042- connecting tube, the first delivery pipe of 1043-, the second delivery pipe of 1044-, 901- ethyl alcohol recycle condenser, 902-
Ethyl alcohol accumulator tank, 903- ethyl alcohol recycle tail condenser, 904- third return pipe, 121- secondary concentration kettle, 122- toluene metal bucket, 123-
Purify reflux condenser, 124- glabridin centrifuge, the second rotary evaporator of 125-, the second return pipe of 126-.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples, but be not intended as to the present invention limit according to
According to.
Embodiment.A kind of environment-friendly type glabridin extraction element is constituted as shown in Figure 1, including ethyl alcohol configuration device 1, second
Multiple glass chromatography columns 3 are connected in alcohol configuration device 1 side by side, each glass chromatography column 3 is connected separately with through the first isocon 4
First chromatography liquid bath 5, second chromatographs liquid bath 6 and third chromatographs liquid bath 7, and the first chromatography liquid bath 5, second chromatographs liquid bath 6 and third
7 outside of chromatography liquid bath is connected separately with the first chromatographic solution concentration kettle 2, the second chromatographic solution concentration kettle through multiple chromatographic solution feed pumps
8 and third chromatographic solution concentration kettle 11, wherein the first chromatographic solution concentration kettle 2 and 8 side of the second chromatographic solution concentration kettle are connected with ethyl alcohol
Recyclable device 9, the other side are connected with the first rotary evaporator 10；11 side of the third chromatographic solution concentration kettle connection ethyl alcohol recycling
Device 9,11 other side of third chromatographic solution concentration kettle are connected with enrichment facility 12, and first rotary evaporator 10 is through the first reflux
Pipe 13 connects alcohol recovering device 9.
The ethyl alcohol configuration device 1 includes ethanol solution make-up tank 101, and 101 side of ethanol solution make-up tank is connected with second
Alcohol storage tank and water pipe, 101 other side of ethanol solution make-up tank are connected separately with the first ethanol solution transfer tank through ethanol solution pump
102 and the second ethanol solution transfer tank 103, connect on the first ethanol solution transfer tank 102 and the second ethanol solution transfer tank 103
Compressed air hose is connect, the first ethanol solution transfer tank 102 and the second ethanol solution transfer tank 103 are distinguished through the second isocon 104
Connect multiple glass chromatography columns 3.
Second isocon 104 includes the multiple branch pipes 1041 being connected on multiple glass chromatography columns 3, every two
It is connected with each other between branch pipe 1041 through connecting tube 1042, the first delivery pipe 1043 and second is connected separately on the outside of connecting tube 1042
Delivery pipe 1044,1043 end of the first delivery pipe connect the first ethanol solution transfer tank 102, the connection of 1044 end of the second delivery pipe
Second ethanol solution transfer tank 103.
The alcohol recovering device 9 includes that three ethyl alcohol arranged side by side recycle condenser 901, three ethyl alcohol recycling condensations
901 side of device is separately connected the first chromatographic solution concentration kettle 2, the second chromatographic solution concentration kettle 8 and third chromatographic solution concentration kettle 11, and three
Ethyl alcohol recycling 901 other side of condenser is respectively connected with ethyl alcohol accumulator tank 902 and ethyl alcohol recycling tail condenser 903, and it is solidifying that ethyl alcohol recycles tail
903 side of device connects ethyl alcohol accumulator tank 902, and 902 outside of ethyl alcohol accumulator tank connects ethyl alcohol configuration device 1 through third return pipe 904.
The enrichment facility 12 includes secondary concentration kettle 121, and 121 side of secondary concentration kettle connects third chromatographic solution concentration kettle
11,121 other side of secondary concentration kettle is connected separately with toluene metal bucket 122, purifying reflux condenser 123 and glabridin centrifuge
124,124 outside of glabridin centrifuge is connected with the second rotary evaporator 125, the second rotary evaporator through device for transporting objects
125 connect ethyl alcohol accumulator tank 902 through the second return pipe 126.
With a kind of glabridin extraction process of the extraction element, comprising the following steps:
1. preparing the ethanol water of 50% concentration in ethanol solution make-up tank, then it is respectively fed to through the second isocon
It is spare in first ethanol solution transfer tank and the second ethanol solution transfer tank, obtain A ethanol solution；
2. the crude flavonoid powder after weighing is respectively put into multiple glass chromatography columns, and it is mixed that polystyrene resin or silica gel is added
It closes uniformly, then removes insoluble impurity, obtain B flavones ethanol solution；
3. B flavones ethanol solution is separated by the polystyrene resin or silica gel being mixed in B flavones ethanol solution,
The glabridin ethyl alcohol water mixed liquid of different purity is obtained, C mixed liquor is obtained；
4. the glabridin content of C mixed liquor in each glass chromatography column is measured respectively by liquid chromatogram, then according to light
Each C mixed liquor is respectively fed in the first chromatography liquid bath, the second chromatography liquid bath and third chromatography liquid bath by the content of licoricidin, wherein
20% glabridin content C mixed liquor below is sent into the first chromatography liquid bath, and the C mixed liquor of 20~40% glabridin contents is sent
Enter the second chromatography liquid bath, more than 40% glabridin content C mixed liquor is sent into third and chromatographs liquid bath, successively obtain D mixed liquor,
E mixed liquor and F mixed liquor；
5. D mixed liquor is sent into the first chromatographic solution concentration kettle and carries out concentration distillation, then vinasse is sent into the first rotation
Turn evaporator for decompression to be evaporated, obtains 20% concentration glabridin powder product below；E mixed liquor is sent into the second chromatographic solution
Concentration distillation is carried out in concentration kettle and obtains f1 concentrate, then dehydrated alcohol dissolved dilution is added into f1 concentrate manually, filtering
After obtain f2 concentrate, then f2 concentrate is sent into evaporated under reduced pressure in the first rotary evaporator, obtains the light of 20~40% concentration
Licoricidin powder product；F mixed liquor is sent into third chromatographic solution concentration kettle and carries out concentration distillation and obtains f3 concentrate, then by f3
Concentrate is sent into enrichment facility and carries out secondary concentration, obtains the glabridin powder product of 90% concentration.
First rotary evaporator to D mixed liquor, E mixed liquor during being evaporated by the ethyl alcohol after evaporation after condensing weight
It is new to be sent into ethyl alcohol accumulator tank, realize the recycling to ethyl alcohol.
Secondary concentration mode of the enrichment facility to f3 concentrate specifically: first press f3 concentrate, acetone and toluene
The mass ratio of 10:5:4 is sent into secondary concentration kettle, and wherein f3 is concentrated by steam heating by direct plungeing into manually in acetone
Liquid, which is dissolved in acetone toluene Mixed Solvent, obtains mixed liquor, then to cooling after mixed liquor insulated and stirred half an hour, makes to mix
The glabridin closed in liquid recrystallizes to form solid, passes through the solvent that purifying reflux condenser will volatilize during insulated and stirred
Direct cooling can be back to again in secondary concentration kettle, guarantee being thoroughly mixed for solute；It is sweet that solid is sent to light after being precipitated again
Grass is determined to be centrifugally separating to obtain filter cake in centrifuge, finally by being sent into the second rotation through device for transporting objects after manually taking out filter cake
Evaporator evaporated under reduced pressure obtains the glabridin powder product of 90% concentration.
Ethyl alcohol after evaporation in being re-fed into f3 mixed liquor by the second rotary evaporator during being evaporated after condensing
In ethyl alcohol accumulator tank, the recycling to ethyl alcohol is realized.
The working principle of the invention: the present invention passes through multiple glass chromatography columns 3 and ethyl alcohol configuration device 1 during the preparation process
Cooperation, dissolution purification can be carried out to more parts of thick brass respectively, so that the flavones ethyl alcohol for obtaining different glabridin concentration is molten
Liquid, by the cooperation of the first isocon 4, each analysis liquid bath 5 and each chromatographic solution concentration kettle, flavones second that can respectively to various concentration
Alcoholic solution carries out following process, so that the powdery glabridin finished product of different content is obtained, to realize to the complete of raw material
It utilizes.Process obtained 40% content or more glabridin mixed liquor can also be carried out by enrichment facility 12 concentration again and
Purification, to obtain the glabridin mixed liquor of 90% content, processing stability is high, and processing effect is good.The concentration of first chromatographic solution
Kettle 2, the second chromatographic solution concentration kettle 8 and third chromatographic solution concentration kettle 11, can be right by alcohol recovering device 9 in concentration process
Ethyl alcohol after evaporation is collected and condensing recovery, and is re-fed into the ethanol solution being collected by third return pipe 904
In ethyl alcohol configuration device 1, the secondary use of right raw material is realized；Pass through the first rotary evaporator 10 and the second rotary evaporator
125 ethanol solutions that can also be will volatilize during being evaporated are collected, are sent into ethyl alcohol accumulator tank 902 after condensation, are further mentioned
The high present invention recycles effect to ethyl alcohol.
Claims (7)
1. a kind of environment-friendly type glabridin extraction element, it is characterised in that: including ethyl alcohol configuration device (1), ethyl alcohol configuration device
(1) it is connected with side by side on multiple glass chromatography columns (3), each glass chromatography column (3) is connected separately with through the first isocon (4)
One chromatography liquid bath (5), the second chromatography liquid bath (6) and third chromatography liquid bath (7), the first chromatography liquid bath (5), the second chromatography liquid bath
(6) and on the outside of third chromatography liquid bath (7) the first chromatographic solution concentration kettle (2), the second chromatographic solution concentration kettle (8) and the are connected separately with
Three chromatographic solution concentration kettles (11), wherein the first chromatographic solution concentration kettle (2) and second chromatographic solution concentration kettle (8) side are connected with ethyl alcohol
Recyclable device (9), the other side are connected with the first rotary evaporator (10)；The third chromatographic solution concentration kettle (11) side connects second
Alcohol recyclable device (9), third chromatographic solution concentration kettle (11) other side are connected with enrichment facility (12), first rotary evaporator
(10) alcohol recovering device (9) are connected through the first return pipe (13).
2. a kind of environment-friendly type glabridin extraction element according to claim 1, it is characterised in that: the ethyl alcohol configuration dress
Setting (1) includes ethanol solution make-up tank (101), is connected separately in the first ethanol solution on the outside of ethanol solution make-up tank (101)
Turn trough (102) and the second ethanol solution transfer tank (103), the first ethanol solution transfer tank (102) and the second ethanol solution transfer
Slot (103) is separately connected multiple glass chromatography columns (3) through the second isocon (104).
3. a kind of environment-friendly type glabridin extraction element according to claim 2, it is characterised in that: second isocon
It (104) include the multiple branch pipes (1041) being connected on multiple glass chromatography columns (3), every two branch pipe passes through between (1041)
Connecting tube (1042) is connected with each other, and is connected separately with the first delivery pipe (1043) and the second delivery pipe on the outside of connecting tube (1042)
(1044), the first delivery pipe (1043) end connects the first ethanol solution transfer tank (102), and the second delivery pipe (1044) end connects
Connect the second ethanol solution transfer tank (103).
4. a kind of environment-friendly type glabridin extraction element according to claim 1, it is characterised in that: the ethyl alcohol recycling dress
Setting (9) includes three ethyl alcohol recycling condenser (901) arranged side by side, and three ethyl alcohol recycling condenser (901) sides connect respectively
Connect the first chromatographic solution concentration kettle (2), the second chromatographic solution concentration kettle (8) and third chromatographic solution concentration kettle (11), three ethyl alcohol recycling
Condenser (901) other side is respectively connected with ethyl alcohol accumulator tank (902) and ethyl alcohol recycling tail condenser (903), and ethyl alcohol recycles tail condenser
(903) side connection ethyl alcohol accumulator tank (902), ethyl alcohol accumulator tank (902) outside is through third return pipe (904) connection ethyl alcohol configuration
Device (1).
5. a kind of environment-friendly type glabridin extraction element according to claim 1, it is characterised in that: the enrichment facility
It (12) include secondary concentration kettle (121), secondary concentration kettle (121) side connects third chromatographic solution concentration kettle (11), secondary concentration
Kettle (121) other side is connected separately with toluene metal bucket (122), purifying reflux condenser (123) and glabridin centrifuge
(124), it is connected with the second rotary evaporator (125) on the outside of glabridin centrifuge (124), the second rotary evaporator (125) warp
Second return pipe (126) connects alcohol recovering device (9).
6. special with a kind of glabridin extraction process of extraction element described in any claim in claim 1-5
Sign is, comprising the following steps:
1. preparing the ethanol water of 50% concentration in ethanol solution make-up tank, first then is respectively fed to through the second isocon
It is spare in ethanol solution transfer tank and the second ethanol solution transfer tank, obtain A ethanol solution；
2. the crude flavonoid powder after weighing is respectively put into multiple glass chromatography columns, and polystyrene resin or silica gel mixing is added
It is even, insoluble impurity is then removed, B flavones ethanol solution is obtained；
3. being separated by the polystyrene resin or silica gel being mixed in B flavones ethanol solution to B flavones ethanol solution, obtain
The glabridin ethyl alcohol water mixed liquid of different purity, obtains C mixed liquor；
4. the C mixed liquor in multiple glass chromatography columns is respectively fed to the first chromatography liquid bath, the second layer by the content of glabridin
It analyses in liquid bath and third chromatography liquid bath, wherein 20% glabridin content the first chromatography of C mixed liquor feeding liquid bath below, 20~
The C mixed liquor of 40% glabridin content is sent into the second chromatography liquid bath, and C mixed liquor more than 40% glabridin content is sent into the
Three chromatography liquid baths, successively obtain D mixed liquor, E mixed liquor and F mixed liquor；
5. D mixed liquor is sent into the first chromatographic solution concentration kettle and carries out concentration distillation, then vinasse is sent into the first rotation and is steamed
Evaporated under reduced pressure in device is sent out, 20% concentration glabridin powder product below is obtained；E mixed liquor is sent into the concentration of the second chromatographic solution
Concentration distillation is carried out in kettle and obtains f1 concentrate, then dehydrated alcohol dissolved dilution is added into f1 concentrate, obtains f2 after filtering
Concentrate, then f2 concentrate is sent into evaporated under reduced pressure in the first rotary evaporator, obtain the glabridin powder of 20~40% concentration
Last finished product；F mixed liquor is sent into third chromatographic solution concentration kettle be concentrated distilling and obtains f3 concentrate, then f3 concentrate is sent
Enter enrichment facility and carry out secondary concentration, obtains the glabridin powder product of 90% concentration.
7. a kind of glabridin extraction process according to claim 6, which is characterized in that f3 is concentrated in the enrichment facility
The secondary concentration mode of liquid specifically: f3 concentrate, acetone and toluene are first sent into secondary concentration kettle by the mass ratio of 10:5:4
In, f3 concentrate is dissolved in acetone toluene Mixed Solvent by steam heating and obtains mixed liquor, after insulated and stirred half an hour
It cools, the glabridin in mixed liquor is made to recrystallize to form solid, then the solid is sent into glabridin centrifuge
It is centrifugally separating to obtain filter cake, filter cake is finally sent into the second rotary evaporator evaporated under reduced pressure, obtains the glabridin of 90% concentration
Powder product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665253A (en) * | 2019-11-04 | 2020-01-10 | 三益创价生物科技(深圳)有限公司 | High-efficiency multifunctional SCF device and consistent operation type multifunctional SCF device |
| CN112724155A (en) * | 2020-12-16 | 2021-04-30 | 洛阳蓝斯利科技有限公司 | Method for preparing white glabridin by subcritical technology |
Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02129198A (en) * | 1988-11-07 | 1990-05-17 | Dowa Mining Co Ltd | Method for recovering saponin from asparagus waste |
| KR20040067022A (en) * | 2003-01-21 | 2004-07-30 | 학교법인 인하학원 | A process of extracting glabridine from licorice root |
| US20050220913A1 (en) * | 2004-03-31 | 2005-10-06 | Council Of Scientific And Industrial Research | Novel in-expensive and efficient process for isolation of imperatorin, a potent inducible nitric oxide synthase inhibitor and anti-inflammatory drug candidate from Aegle marmelos Correa |
| CN101139269A (en) * | 2007-08-30 | 2008-03-12 | 季萍 | Method for producing male contraceptive raw material medicine-gossypol acetate |
| CN201249052Y (en) * | 2008-08-02 | 2009-06-03 | 温州市金榜轻工机械有限公司 | Full-automatic chromatographic separator set |
| CN101735233A (en) * | 2009-12-11 | 2010-06-16 | 暨南大学 | Method for producing high-purity glabridin |
| CN101830906A (en) * | 2009-12-13 | 2010-09-15 | 成都普思生物科技有限公司 | Separation and purification method of high-purity glabridin |
| CN202901832U (en) * | 2012-12-03 | 2013-04-24 | 浙江嘉利珂钴镍材料有限公司 | Liquid-state SO2 conveyer device for continuous liquid-state SO2 vaporization system |
| CN203107747U (en) * | 2013-01-30 | 2013-08-07 | 山东贝隆杜仲生物工程有限公司 | Folium cortex eucommiae extraction device provided with solvent recovery system |
| WO2014094405A1 (en) * | 2012-12-17 | 2014-06-26 | 石家庄市兴柏生物工程有限公司 | Method for extraction and preparation of avermectin b2a |
| CN104906144A (en) * | 2015-05-20 | 2015-09-16 | 哈尔滨工业大学 | System and method for controlling bioactivator separation and purification process |
| CN106166403A (en) * | 2016-08-28 | 2016-11-30 | 云南品益生物科技有限公司 | Automatic chromatographic apparatus and method are organized into groups in circulation |
| CN106349737A (en) * | 2016-08-10 | 2017-01-25 | 姚树明 | Preparation method of Salvia japonica Thunb. vegetable dye |
| CN108176079A (en) * | 2017-12-29 | 2018-06-19 | 无限极（中国）有限公司 | A kind of discoloration method of licorice |
| CN108822164A (en) * | 2018-05-23 | 2018-11-16 | 海南益尔生物制药有限公司 | The preparation process of high quality monosialotetrahexose ganglioside sodium |
| CN209361901U (en) * | 2019-01-03 | 2019-09-10 | 湖州欧利生物科技有限公司 | Environment-friendly type glabridin extraction element |
-
2019
- 2019-01-03 CN CN201910003005.2A patent/CN109395427A/en active Pending
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02129198A (en) * | 1988-11-07 | 1990-05-17 | Dowa Mining Co Ltd | Method for recovering saponin from asparagus waste |
| KR20040067022A (en) * | 2003-01-21 | 2004-07-30 | 학교법인 인하학원 | A process of extracting glabridine from licorice root |
| US20050220913A1 (en) * | 2004-03-31 | 2005-10-06 | Council Of Scientific And Industrial Research | Novel in-expensive and efficient process for isolation of imperatorin, a potent inducible nitric oxide synthase inhibitor and anti-inflammatory drug candidate from Aegle marmelos Correa |
| CN101139269A (en) * | 2007-08-30 | 2008-03-12 | 季萍 | Method for producing male contraceptive raw material medicine-gossypol acetate |
| CN201249052Y (en) * | 2008-08-02 | 2009-06-03 | 温州市金榜轻工机械有限公司 | Full-automatic chromatographic separator set |
| CN101735233A (en) * | 2009-12-11 | 2010-06-16 | 暨南大学 | Method for producing high-purity glabridin |
| CN101830906A (en) * | 2009-12-13 | 2010-09-15 | 成都普思生物科技有限公司 | Separation and purification method of high-purity glabridin |
| CN202901832U (en) * | 2012-12-03 | 2013-04-24 | 浙江嘉利珂钴镍材料有限公司 | Liquid-state SO2 conveyer device for continuous liquid-state SO2 vaporization system |
| WO2014094405A1 (en) * | 2012-12-17 | 2014-06-26 | 石家庄市兴柏生物工程有限公司 | Method for extraction and preparation of avermectin b2a |
| CN203107747U (en) * | 2013-01-30 | 2013-08-07 | 山东贝隆杜仲生物工程有限公司 | Folium cortex eucommiae extraction device provided with solvent recovery system |
| CN104906144A (en) * | 2015-05-20 | 2015-09-16 | 哈尔滨工业大学 | System and method for controlling bioactivator separation and purification process |
| CN106349737A (en) * | 2016-08-10 | 2017-01-25 | 姚树明 | Preparation method of Salvia japonica Thunb. vegetable dye |
| CN106166403A (en) * | 2016-08-28 | 2016-11-30 | 云南品益生物科技有限公司 | Automatic chromatographic apparatus and method are organized into groups in circulation |
| CN108176079A (en) * | 2017-12-29 | 2018-06-19 | 无限极（中国）有限公司 | A kind of discoloration method of licorice |
| CN108822164A (en) * | 2018-05-23 | 2018-11-16 | 海南益尔生物制药有限公司 | The preparation process of high quality monosialotetrahexose ganglioside sodium |
| CN209361901U (en) * | 2019-01-03 | 2019-09-10 | 湖州欧利生物科技有限公司 | Environment-friendly type glabridin extraction element |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665253A (en) * | 2019-11-04 | 2020-01-10 | 三益创价生物科技(深圳)有限公司 | High-efficiency multifunctional SCF device and consistent operation type multifunctional SCF device |
| CN110665253B (en) * | 2019-11-04 | 2021-04-06 | 三益创价生物科技(深圳)有限公司 | High-efficiency multifunctional SCF device and consistent operation type multifunctional SCF device |
| CN112724155A (en) * | 2020-12-16 | 2021-04-30 | 洛阳蓝斯利科技有限公司 | Method for preparing white glabridin by subcritical technology |
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