CN110270134A - A kind of high-purity C BD isolates and purifies device and its isolation and purification method - Google Patents
A kind of high-purity C BD isolates and purifies device and its isolation and purification method Download PDFInfo
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- CN110270134A CN110270134A CN201910685993.3A CN201910685993A CN110270134A CN 110270134 A CN110270134 A CN 110270134A CN 201910685993 A CN201910685993 A CN 201910685993A CN 110270134 A CN110270134 A CN 110270134A
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- 238000000034 method Methods 0.000 title claims description 21
- 238000000746 purification Methods 0.000 title claims description 16
- 238000002955 isolation Methods 0.000 title claims description 14
- 239000003480 eluent Substances 0.000 claims abstract description 159
- 239000006227 byproduct Substances 0.000 claims abstract description 52
- 239000007788 liquid Substances 0.000 claims abstract description 45
- 238000010828 elution Methods 0.000 claims abstract description 19
- 239000000284 extract Substances 0.000 claims abstract description 6
- 239000012190 activator Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 230000005526 G1 to G0 transition Effects 0.000 claims description 22
- 238000011001 backwashing Methods 0.000 claims description 19
- 239000000047 product Substances 0.000 claims description 11
- 239000000872 buffer Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000007790 solid phase Substances 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 238000011144 upstream manufacturing Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- -1 third eluant Substances 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 3
- 238000004587 chromatography analysis Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 230000003139 buffering effect Effects 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- QHMBSVQNZZTUGM-UHFFFAOYSA-N Trans-Cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-UHFFFAOYSA-N 0.000 description 81
- QHMBSVQNZZTUGM-ZWKOTPCHSA-N cannabidiol Chemical compound OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-ZWKOTPCHSA-N 0.000 description 81
- 229950011318 cannabidiol Drugs 0.000 description 81
- ZTGXAWYVTLUPDT-UHFFFAOYSA-N cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CC=C(C)C1 ZTGXAWYVTLUPDT-UHFFFAOYSA-N 0.000 description 81
- PCXRACLQFPRCBB-ZWKOTPCHSA-N dihydrocannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)C)CCC(C)=C1 PCXRACLQFPRCBB-ZWKOTPCHSA-N 0.000 description 81
- 230000000694 effects Effects 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 241000218236 Cannabis Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- CYQFCXCEBYINGO-UHFFFAOYSA-N THC Natural products C1=C(C)CCC2C(C)(C)OC3=CC(CCCCC)=CC(O)=C3C21 CYQFCXCEBYINGO-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- CYQFCXCEBYINGO-IAGOWNOFSA-N delta1-THC Chemical compound C1=C(C)CC[C@H]2C(C)(C)OC3=CC(CCCCC)=CC(O)=C3[C@@H]21 CYQFCXCEBYINGO-IAGOWNOFSA-N 0.000 description 2
- 229960004242 dronabinol Drugs 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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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
- B01D15/42—Selective adsorption, e.g. chromatography characterised by the development mode, e.g. by displacement or by elution
- B01D15/424—Elution mode
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses a kind of high-purity C BD to isolate and purify device, including at least a set of level-one chromatographic column and second level chromatographic column, level-one eluant, eluent entrance is provided at the top of level-one chromatographic column, the bottom of level-one chromatographic column connects level-one discharge pipe, level-one eluant, eluent is arranged on level-one discharge pipe to export, first byproduct discharge, second byproduct discharge and the outlet of the first CBD liquid, first detector is set on level-one discharge pipe, second level elution pipeline is connected at the top of the outlet of first CBD liquid and second level chromatographic column, second level elution pipeline is provided with constant flow pump, second level discharge pipe is arranged in second level chromatographic column bottom and top, second level eluant, eluent entrance, second level discharge pipe is arranged second level eluant, eluent and exports, third byproduct discharge and the outlet of the 2nd CBD liquid, the second detector is arranged in second level discharge pipe, level-one eluant, eluent entrance by first into Pipe material extracts liquid storage tank, the first eluant, eluent storage tank, the second eluant, eluent storage tank with CBD respectively and is connected, and improves purity.
Description
Technical field
The present invention relates to a kind of high-purity C BD to isolate and purify device, also relates to point that device is isolated and purified using this
From purification process.
Background technique
Cannabidiol (CBD), a kind of cannboid found in cannabis plants, as a kind of common disease for the treatment of
Alternative solution is becoming increasingly popular.Different from another cannboid tetrahydrocannabinol (THC) found in cannabis plants, CBD does not have
There is mentation.However, only 20% is absorbed, it means that make CBD more efficient, it is necessary to execute when taking in CBD
The extraction of CBD separates.Not high enough for the target product CBD purity obtained after the isolating and purifying of CBD at present thus current
It needs further to be isolated and purified in the extraction process of CBD.
Summary of the invention
The technical problems to be solved by the present invention are: providing a kind of high-purity C BD isolates and purifies device, this isolates and purifies dress
It sets by isolating and purifying effect twice, to improve the purity of target product CBD.
Another technical problem to be solved by this invention is: providing a kind of high-purity C BD isolation and purification method, the separation
Purification process is isolated and purified effect by isolating and purifying device twice, to improve the purity of target product CBD.
In order to solve the first technical problem mentioned above, the technical scheme is that a kind of high-purity C BD isolates and purifies dress
It sets, including matching used at least a set of level-one chromatographic column and second level chromatographic column, is all provided in level-one chromatographic column and second level chromatographic column
It is equipped with chromatography solid phase, level-one eluant, eluent entrance is provided at the top of level-one chromatographic column, the bottom of level-one chromatographic column is connected with level-one
Discharge pipe, be provided on the level-one discharge pipe outlet of level-one eluant, eluent, the first byproduct discharge, the second byproduct discharge and
The outlet of first CBD liquid, is provided with the first detector for detecting internal flow liquid color on level-one discharge pipe, and described the
The outlet of one CBD liquid is connected to at the top of second level chromatographic column by second level elution pipeline, is provided with constant flow pump on second level elution pipeline；
The bottom of the second level chromatographic column is provided with second level discharge pipe, is provided with second level eluant, eluent at the top of the second level chromatographic column and enters
Mouthful, it is provided with the outlet of second level eluant, eluent, third byproduct discharge and the outlet of the 2nd CBD liquid, second level on the second level discharge pipe and goes out
The second detector for detecting internal flow material color is provided on pipe material；The level-one eluant, eluent entrance passes through first
Feed pipe extracts liquid storage tank, the first eluant, eluent storage tank, the second eluant, eluent storage tank with CBD respectively and is connected, the second level elution
Agent entrance is connected to third eluant, eluent storage tank and the 4th eluant, eluent storage tank respectively by the second feed pipe.
As a preferred solution, the first distributor and are respectively arranged on the first feed pipe and the second feed pipe
Two distributors, the level-one eluant, eluent entrance of the level-one chromatographic column pass through the first parallel pipeline with the outlet of the first distributor respectively
Connection, the second level eluant, eluent entrance of the second level chromatographic column are connected with the outlet of the second distributor by the second parallel pipeline respectively
It is logical, inlet control valve is provided on the first parallel pipeline and the second parallel pipeline.
As a preferred solution, activator is provided at the top of the level-one chromatographic column and second level chromatographic column to enter
Mouthful, bottom is provided with activator outlet, and activator entrance connects activator supply line, activator outlet connection activator reflux
Pipeline.
As a preferred solution, the bottom of the level-one chromatographic column and second level chromatographic column is provided with backwashing water and enters
Mouthful, top is provided with backwashing water outlet, the backwashing water entrance and pure water rinsing piping connection, and backwashing water outlet divides company
It connects in blowoff line.
As a preferred solution, first feed pipe and the second feed pipe are provided with mass flow meters, the
Shunting meter is provided on one parallel pipeline and the second parallel pipeline.
As a preferred solution, the upstream for constant flow pump being located on second level elution pipeline is provided with buffer.
After above-mentioned technical proposal, effect of the invention is: this isolates and purifies first into level-one chromatographic column in device
After be passed through the first eluant, eluent, the second eluant, eluent, so as to be extracted target product CBD after continuously first having eluted by-product,
The concentration of CBD at this time is not high, and the inside may be contained not by isolated by-product, therefore eluent is re-introduced into second level layer
Secondary elution is carried out in analysis column, by-product is eluted more thoroughly and is separated with CBD, to improve the purity of CBD.
In addition, being provided with activator entrance at the top of the level-one chromatographic column and second level chromatographic column, bottom is provided with work
Agent outlet, activator entrance connect activator supply line, and activator outlet connection activator reflux line in this way can be right
Solid phase in level-one chromatographic column and second level chromatographic column is activated, it is ensured that solid phase can for a long time effectively.
And the first distributor and the second distributor are respectively arranged on the first feed pipe and the second feed pipe, the level-one
The level-one eluant, eluent entrance of chromatographic column is connected to the outlet of the first distributor by the first parallel pipeline, the second level chromatographic column
Second level eluant, eluent entrance is connected to the outlet of the second distributor by the second parallel pipeline, the first parallel pipeline and the second parallel transistor
It is provided with inlet control valve on road, more accurately can quantitatively be divided equally eluant, eluent, CBD extracting solution using two distributors
To each level-one chromatographic column and second level chromatographic column, the dosage of such eluant, eluent more preferably controls, avoids wasting.
And the bottom of the level-one chromatographic column and second level chromatographic column is provided with backwashing water entrance, top is provided with recoil
Washing water outlet, the backwashing water entrance and pure water rinsing piping connection, backwashing water outlet point connect in blowoff line, in this way
It can use pure water to backwash level-one chromatographic column and second level chromatographic column, avoid internal solid phase hardened.
To solve above-mentioned second technical problem, the technical scheme is that a kind of side of isolating and purifying high-purity C BD
Method, the isolation and purification method used it is above-mentioned isolate and purify device, which includes
S1, preparation stage
A class stationary phase is added into level-one chromatographic column, B class stationary phase is added in second level chromatographic column, CBD extracting solution is added to
CBD extracts liquid storage tank；The first deployed eluant, eluent, the second eluant, eluent, third eluant, eluent, the 4th eluant, eluent are separately added into phase
In corresponding basin；Wherein the affinity of the first eluant, eluent and the by-product in CBD extracting solution is greater than by-product and A class stationary phase
Affinity, the affinity of the CBD in the first eluant, eluent and CBD extracting solution is less than the affinity of CBD and A class stationary phase；Second
The affinity of CBD in eluant, eluent and CBD extracting solution is greater than the affinity of CBD and A class stationary phase；Third eluant, eluent is mentioned with CBD
Take the affinity of the by-product in liquid greater than the affinity of by-product and B class stationary phase, the affinity of third eluant, eluent and CBD are small
In the affinity of CBD and B class stationary phase；The affinity of 4th eluant, eluent and the CBD in CBD extracting solution are greater than CBD and B class and fix
The affinity of phase；
S2, level-one isolate and purify；
CBD extracting solution is quantitatively adding in level-one chromatographic column, to CBD extracting solution addition after, by the first eluant, eluent,
Second eluant, eluent is successively quantitatively adding progress level-one in level-one chromatographic column and isolates and purifies, and passes through the first detector and detects eluent
Color, according to testing result corresponding eluant component difference respectively from the outlet of level-one eluant, eluent, the first byproduct discharge,
Second byproduct discharge and the first CBD liquid outlet export；
S3, the second-order separation purifying；
Eluent after level-one isolates and purifies quantitatively is flowed into second level chromatographic column from the outlet of the first CBD liquid carries out two
Grade isolates and purifies, and the color of eluent is detected by the second detector, and corresponding eluant component is different according to testing result
Respectively from the outlet of second level eluant, eluent, third byproduct discharge and the 2nd CBD liquid outlet export.
It is further preferred that adding the first eluant, eluent persistently during step S2 level-one isolates and purifies to successively
It elutes the first by-product and exports it from the first byproduct discharge, elute the second by-product and lead it from the second byproduct discharge
Out, then according to the first detector detect level-one chromatographic column in derived eluent be the first eluant, eluent when, the first eluant, eluent from
The outlet of level-one eluant, eluent is exported and is branched in the first elution return tank；Hereafter stop the first eluant, eluent of supply to transfer to continue addition
Target product CBD is eluted and is exported from the first CBD liquid and exported by the second eluant, eluent, the second eluant, eluent, and when the first detector is examined
When derived eluent is the second eluant, eluent in survey level-one chromatographic column, the second eluant, eluent exports from level-one eluant, eluent and exports and shunt
Into the second elution return tank.
It is further preferred that the isolation and purification method further includes the rationed method of CBD extracting solution and eluant, eluent:
Wherein CBD extracting solution, the first eluant, eluent, the second eluant, eluent are introduced into first before entering level-one chromatographic column
In distributor, the total flow Q1 entered in the first distributor is detected by mass flow meters, then the first distributor same time-division
The level-one chromatographic column of the N number of parallel connection of dispensing, each level-one chromatographic column are all connected with a shunting meter, shunt meter monitoring and are flowed into one
The shunt volume q1, Q1=Nq1 of liquid in grade chromatographic column；Equally, the second distributor is arranged in the upstream of second level chromatographic column, passes through
Second distributor distributes to the second level chromatographic column of N number of parallel connection simultaneously, the total flow of the influent by monitoring the second distributor
The flow that each second level chromatographic column is controlled with the shunt volume in single second level chromatographic column is equal.
It is further preferred that the target product CBD of level-one chromatographic column effluent passes through constant current after first passing through buffer buffering again
Pump is quantitatively sent to second level chromatographic column.
After above-mentioned technical proposal, effect of the invention is: the isolation and purification method elder generation level-one chromatographic column elutes
Target product CBD is extracted after by-product, then eluent, which is re-introduced into second level chromatographic column, carries out secondary elution, and making in this way can
To improve the purity of CBD.
The reflux of the first eluant, eluent, the second eluant, eluent may be implemented in this method using the first detector, so that first washes
De- agent and the second eluant, eluent can be utilized again, avoid wasting.
In this method by the first distributor, the second distributor, mass flow meters, respectively to shunt meter, buffer, constant flow pump total
Same-action, each level-one column flow is all the same, and each second level column flow is all the same, therefore can preferably control each
The dosage of eluant, eluent.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is the schematic diagram of the embodiment of the present invention；
In attached drawing: 1. level-one chromatographic columns；2. second level chromatographic column；3. level-one eluant, eluent entrance；4. level-one discharge pipe；5. one
The outlet of grade eluant, eluent；6. the first byproduct discharge；7. the second byproduct discharge；8. the first CBD liquid exports；9. the first detector；
10. second level elutes pipeline；11. constant flow pump；12. second level discharge pipe；13. second level eluant, eluent entrance；14. second level eluant, eluent goes out
Mouthful；15. third byproduct discharge；16. the 2nd CBD liquid exports；17. the second detector；18. the first feed pipe；19.CBD is mentioned
Take liquid storage tank；20. the first eluant, eluent storage tank；21. the second eluant, eluent storage tank；22. the second feed pipe；23. third eluant, eluent stores up
Tank；24. the 4th eluant, eluent storage tank；25. the first distributor；26. the second distributor；27. the first parallel pipeline；28. second is in parallel
Pipeline；29. inlet control valve；30. activator entrance；31. activator exports；32. backwashing water entrance；33. backwashing water goes out
Mouthful；34. mass flow meters；35. shunting meter；36. buffer.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail.
As shown in Figure 1, a kind of high-purity C BD isolates and purifies device, including matching used at least a set of level-one chromatographic column 1
With second level chromatographic column 2, chromatography solid phase is provided in level-one chromatographic column 1 and second level chromatographic column 2, the top of level-one chromatographic column 1 is set
It is equipped with level-one eluant, eluent entrance 3, the bottom of level-one chromatographic column 1 is connected with level-one discharge pipe 4, sets on the level-one discharge pipe 4
It is equipped with level-one eluant, eluent and exports the 5, first byproduct discharge 6, the second byproduct discharge 7 and the first CBD liquid outlet 8, level-one discharging
The first detector 9 for detecting internal flow liquid color, the first CBD liquid outlet 8 and second level chromatographic column are provided on pipeline 4
2 tops elute pipeline 10 by second level and are connected to, and are provided with constant flow pump 11 on second level elution pipeline 10；The second level chromatographic column 2
Bottom be provided with second level discharge pipe 12, the top of second level chromatographic column 2 is provided with second level eluant, eluent entrance 13, second level discharging
Second level eluant, eluent outlet 14, third byproduct discharge 15 and the 2nd CBD liquid outlet 16, second level discharge pipe are provided on pipeline 12
The second detector 17 for detecting internal flow material color is provided on 12；Level-one eluant, eluent entrance 3 passes through the first charging
Pipeline 18 extracts liquid storage tank 19, the first eluant, eluent storage tank 20, the second eluant, eluent storage tank 21 with CBD respectively and is connected, the second level
Eluant, eluent entrance 13 is connected to third eluant, eluent storage tank 23 and the 4th eluant, eluent storage tank 24 respectively by the second feed pipe 22.
In the present embodiment, level-one chromatographic column 1 and second level chromatographic column 2 are three sets, install A class in level-one chromatographic column 1 additional and fix
Phase installs B class stationary phase in second level chromatographic column 2 additional, is respectively arranged with the first distribution on the first feed pipe 18 and the second feed pipe
Device 25 and the second distributor 26, outlet of the level-one eluant, eluent entrance 3 of each level-one chromatographic column 1 respectively with the first distributor 25 pass through
The connection of first parallel pipeline 27, the second level eluant, eluent entrance 13 of each second level chromatographic column 2 are logical with the outlet of the second distributor 26 respectively
The connection of the second parallel pipeline 28 is crossed, is provided with inlet control valve 29 on the first parallel pipeline 27 and the second parallel pipeline 28.When
So, the number of level-one chromatographic column 1 and second level chromatographic column 2 can be controlled according to customer demand.
In the present embodiment, the top of level-one chromatographic column 1 and second level chromatographic column 2 is provided with activator entrance 30, and bottom is set
It is equipped with activator outlet 31, activator entrance 30 connects activator supply line, 31 connection activator return pipe of activator outlet
The bottom of road, level-one chromatographic column 1 and second level chromatographic column 2 is provided with backwashing water entrance 32, and top is provided with backwashing water and goes out
Mouth 33, the backwashing water entrance 32 and pure water rinsing piping connection, 33 connection blowoff lines of backwashing water outlet, the first charging
Pipeline 18 and the second feed pipe 22 are provided with mass flow meters 34, are all provided on the first parallel pipeline 27 and the second parallel pipeline 28
It is equipped with and shunts meter 35, the upstream that constant flow pump 11 is located on second level elution pipeline 10 is provided with buffer 36.
A kind of high-purity C BD isolation and purification method, the method use the above-mentioned devices that isolates and purifies, including S1, preparation
Stage, A class stationary phase was added into level-one chromatographic column 1, B class stationary phase was added in second level chromatographic column 2, CBD extracting solution is added to
CBD extracts liquid storage tank 19；The first deployed eluant, eluent, the second eluant, eluent, third eluant, eluent, the 4th eluant, eluent are separately added into
In corresponding basin；Wherein the affinity of the first eluant, eluent and the by-product in CBD extracting solution is greater than by-product and fixes with A class
The affinity of CBD in the affinity of phase, the first eluant, eluent and CBD extracting solution is less than the affinity of CBD and A class stationary phase；The
The affinity of CBD in two eluant, eluents and CBD extracting solution is greater than the affinity of CBD and A class stationary phase；Third eluant, eluent and CBD
The affinity of by-product in extracting solution is greater than the affinity of by-product and B class stationary phase, the affinity of third eluant, eluent and CBD
Less than the affinity of CBD and B class stationary phase；The affinity of CBD in 4th eluant, eluent and CBD extracting solution is greater than CBD and B class is solid
Determine the affinity of phase；
S2, level-one, which isolate and purify, is quantitatively adding CBD extracting solution in level-one chromatographic column 1, to the end of the addition of CBD extracting solution
Afterwards, the first eluant, eluent, the second eluant, eluent are successively quantitatively adding in level-one chromatographic column 1 and carry out level-one and isolates and purifies, by the
One detector 9 detects the color of eluent, and corresponding eluant component difference is respectively from level-one eluant, eluent according to testing result
Export 8 export of the 5, first byproduct discharge 6, the second byproduct discharge 7 and the outlet of the first CBD liquid；Wherein, persistently addition first is washed
De- agent, successively eluting the first by-product exports it from the first byproduct discharge 6, elutes the second by-product and make it from the second by-product
7 export of object outlet, when then detecting that derived eluent is the first eluant, eluent in level-one chromatographic column 1 according to the first detector 9, the
One eluant, eluent is exported from level-one eluant, eluent outlet 5 and is branched in the first elution return tank；Hereafter stop that the first eluant, eluent is added
Then the second eluant, eluent is persistently added, target product CBD is eluted and from 8 export of the first CBD liquid outlet by the second eluant, eluent, and is worked as
When first detector 9 detects that derived eluent is the second eluant, eluent in level-one chromatographic column 1, the second eluant, eluent is from level-one eluant, eluent
Outlet 5 is exported and is branched in the second elution return tank.
S3, eluent of the second-order separation purifying after level-one isolates and purifies quantitatively are flowed into two from the first CBD liquid outlet 8
The second-order separation purifying is carried out in grade chromatographic column 2, third eluant, eluent, the 4th eluant, eluent are successively quantitatively adding in second level chromatographic column 2,
The color of eluent is detected by the second detector 17, corresponding eluant component difference is respectively from second level according to testing result
Eluant, eluent outlet 14, third byproduct discharge 15 and the 2nd CBD liquid outlet 16 export, and CBD derived from the 2nd CBD liquid outlet 16 is
For the CBD of high-purity.
In the present embodiment, CBD extracting solution, the first eluant, eluent, the second eluant, eluent are advanced before entering level-one chromatographic column 1
Enter into the first distributor 25, the total flow Q1 entered in the first distributor 25 is detected by mass flow meters 34, then
One distributor 25 distributes to three level-one chromatographic columns 1 in parallel simultaneously, and each level-one chromatographic column 1 is all connected with a shunting meter
35, shunt shunt volume q1, Q1=3q1 that meter 35 monitors the liquid being flowed into level-one chromatographic column 1；Equally, second level chromatographs
The second distributor 26 is arranged in the upstream of column 2, distributes to 3 second level chromatographic columns 2 in parallel simultaneously by the second distributor 26, passes through
The shunt volume in the total flow and single second level chromatographic column 2 of the influent of the second distributor 26 is monitored to control each second level layer
The flow of analysis column 2 is equal, and the target product CBD that level-one chromatographic column 1 flows out is first passed through after buffer 36 buffers passes through constant current again
Pump 11 is quantitatively sent to second level chromatographic column 2.
In the present embodiment, the first eluant, eluent and third eluant, eluent can select water, and the second eluant, eluent and the 4th eluant, eluent can
To select alcohol, the second eluant, eluent and the 4th eluant, eluent can choose the alcohol of various concentration according to different requirements,.This implementation
Activator used in example is lye.
After isolating and purifying a period of time, alkali can be added from the activator entrance 30 of level-one chromatographic column 1, second level chromatographic column 2
Liquid is flowed through from 31 outflow of activator outlet after level-one chromatographic column 1, second level chromatographic column 2, then according to circumstances from level-one chromatographic column 1,
Acid solution is added in the activator entrance 30 of second level chromatographic column 2, neutralizes extra alkali after flowing through level-one chromatographic column 1, second level chromatographic column 2
Liquid, from 31 outflow of activator outlet.Then, it is added from backwashing water entrance 32 into level-one chromatographic column 1, second level chromatographic column 2 anti-
Flushing water completes backwash to level-one chromatographic column 1, second level chromatographic column 2 from 33 outflow of backwashing water outlet, thus keep compared with
Good chromatographic effect extends the service life of level-one chromatographic column 1, second level chromatographic column 2.
Embodiment described above is only the description to the preferred embodiment of the present invention, not as the limit to the scope of the invention
It is fixed, on the basis of not departing from design spirit of the present invention, to various modifications and transformation that technical solution of the present invention is made, it should all fall
Enter in the protection scope that claims of the present invention determines.
Claims (10)
1. a kind of high-purity C BD isolates and purifies device, it is characterised in that: including matching used at least a set of level-one chromatographic column and
It is provided with chromatography solid phase in second level chromatographic column, level-one chromatographic column and second level chromatographic column, is provided with one at the top of level-one chromatographic column
Grade eluant, eluent entrance, the bottom of level-one chromatographic column is connected with level-one discharge pipe, is provided with level-one on the level-one discharge pipe and washes
De- agent outlet, the first byproduct discharge, the second byproduct discharge and the first CBD liquid export, and are arranged on level-one discharge pipe useful
Pass through second level at the top of the first detector of detection internal flow liquid color, the first CBD liquid outlet and second level chromatographic column
Pipeline connection is eluted, is provided with constant flow pump on second level elution pipeline；The bottom of the second level chromatographic column is provided with second level discharging
Pipeline is provided with second level eluant, eluent entrance at the top of the second level chromatographic column, and second level elution is provided on the second level discharge pipe
Agent outlet, third byproduct discharge and the 2nd CBD liquid export, and are provided on second level discharge pipe for detecting internal flow substance
Second detector of color；The level-one eluant, eluent entrance is washed with CBD extraction liquid storage tank, first respectively by the first feed pipe
De- agent storage tank, the second eluant, eluent storage tank are connected, and the second level eluant, eluent entrance is washed with third respectively by the second feed pipe
De- agent storage tank and the connection of the 4th eluant, eluent storage tank.
2. a kind of high-purity C BD as described in claim 1 isolates and purifies device, it is characterised in that: the first feed pipe and the
The first distributor and the second distributor, the level-one eluant, eluent entrance difference of the level-one chromatographic column are respectively arranged on two feed pipes
It is connected to the outlet of the first distributor by the first parallel pipeline, the second level eluant, eluent entrance of the second level chromatographic column is respectively with
The outlet of two distributors is connected to by the second parallel pipeline, and charging control is provided on the first parallel pipeline and the second parallel pipeline
Valve processed.
3. a kind of high-purity C BD as claimed in claim 2 isolates and purifies device, it is characterised in that: the level-one chromatographic column and
Activator entrance is provided at the top of second level chromatographic column, bottom is provided with activator outlet, and activator entrance connects activator
Supply line, activator outlet connection activator reflux line.
4. a kind of high-purity C BD as claimed in claim 3 isolates and purifies device, it is characterised in that: the level-one chromatographic column and
The bottom of second level chromatographic column is provided with backwashing water entrance, and top is provided with backwashing water outlet, the backwashing water entrance
With pure water rinsing piping connection, backwashing water outlet point is connected in blowoff line.
5. a kind of high-purity C BD as claimed in claim 4 isolates and purifies device, it is characterised in that: first feed pipe
Mass flow meters are provided with the second feed pipe, are provided with shunting meter on the first parallel pipeline and the second parallel pipeline.
6. a kind of high-purity C BD as claimed in claim 5 isolates and purifies device, it is characterised in that: it is upper that second level elutes pipeline
The upstream of constant flow pump is provided with buffer.
7. a kind of high-purity C BD isolation and purification method, it is characterised in that: the isolation and purification method has used above-mentioned isolate and purify
Device, the isolation and purification method include
S1, preparation stage
A class stationary phase is added into level-one chromatographic column, B class stationary phase is added in second level chromatographic column, CBD extracting solution is added to CBD
Extract liquid storage tank；The first deployed eluant, eluent, the second eluant, eluent, third eluant, eluent, the 4th eluant, eluent are separately added into relatively
In the basin answered；Wherein the affinity of the first eluant, eluent and the by-product in CBD extracting solution is greater than by-product and A class stationary phase
The affinity of CBD in affinity, the first eluant, eluent and CBD extracting solution is less than the affinity of CBD and A class stationary phase；Second washes
The affinity of de- agent and the CBD in CBD extracting solution are greater than the affinity of CBD and A class stationary phase；Third eluant, eluent and CBD are extracted
The affinity of by-product in liquid is greater than the affinity of by-product and B class stationary phase, and the affinity of third eluant, eluent and CBD are less than
The affinity of CBD and B class stationary phase；The affinity of CBD in 4th eluant, eluent and CBD extracting solution is greater than CBD and B class stationary phase
Affinity；
S2, level-one isolate and purify
CBD extracting solution is quantitatively adding in level-one chromatographic column, after being added to CBD extracting solution, by the first eluant, eluent, second
Eluant, eluent is successively quantitatively adding progress level-one in level-one chromatographic column and isolates and purifies, and passes through the face that the first detector detects eluent
Color, corresponding eluant component difference is respectively from the outlet of level-one eluant, eluent, the first byproduct discharge, second according to testing result
Byproduct discharge and the first CBD liquid outlet export；
S3, the second-order separation purifying
Eluent after level-one isolates and purifies quantitatively is flowed into second level chromatographic column from the outlet of the first CBD liquid carries out two fractions
From purifying, the color of eluent is detected by the second detector, according to testing result corresponding eluant component difference difference
From the outlet of second level eluant, eluent, third byproduct discharge and the 2nd CBD liquid outlet export.
8. a kind of high-purity C BD isolation and purification method as claimed in claim 7, it is characterised in that: separated in step S2 level-one
During purifying, persistently adding the first eluant, eluent leads it from the first byproduct discharge to successively elute the first by-product
Out, the second by-product of elution exports it from the second byproduct discharge, is then detected in level-one chromatographic column according to the first detector
When derived eluent is the first eluant, eluent, the first eluant, eluent is exported from level-one eluant, eluent exports and branches to the first elution reflux
In tank；Hereafter stop the first eluant, eluent of supply to transfer to continue the second eluant, eluent of addition, the second eluant, eluent elutes target product CBD
And export and export from the first CBD liquid, and be the second eluant, eluent when the first detector detects derived eluent in level-one chromatographic column
When, the second eluant, eluent exports from level-one eluant, eluent and exports and branch in the second elution return tank.
9. a kind of high-purity C BD isolation and purification method as claimed in claim 8, it is characterised in that: the isolation and purification method
Further include the rationed method of CBD extracting solution and eluant, eluent:
Wherein CBD extracting solution, the first eluant, eluent, the second eluant, eluent are introduced into the first distribution before entering level-one chromatographic column
In device, the total flow Q1 entered in the first distributor is detected by mass flow meters, then the first distributor distributes to N simultaneously
The level-one chromatographic column of a parallel connection, each level-one chromatographic column are all connected with a shunting meter, shunt meter monitoring and are flowed into level-one layer
Analyse the shunt volume q1, Q1=Nq1 of the liquid in column；Equally, the second distributor is arranged in the upstream of second level chromatographic column, passes through second
Distributor distributes to the second level chromatographic column of N number of parallel connection simultaneously, the total flow and list of the influent by monitoring the second distributor
Shunt volume in a second level chromatographic column is equal to control the flow of each second level chromatographic column.
10. a kind of high-purity C BD isolation and purification method as claimed in claim 9, it is characterised in that: level-one chromatographic column effluent
Target product CBD is quantitatively sent by constant flow pump to second level chromatographic column again after first passing through buffer buffering.
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