CN108254475A - A kind of high-speed counter-current chromatograph and method of work for complex sample multi-cycle separation - Google Patents
A kind of high-speed counter-current chromatograph and method of work for complex sample multi-cycle separation Download PDFInfo
- Publication number
- CN108254475A CN108254475A CN201810194444.1A CN201810194444A CN108254475A CN 108254475 A CN108254475 A CN 108254475A CN 201810194444 A CN201810194444 A CN 201810194444A CN 108254475 A CN108254475 A CN 108254475A
- Authority
- CN
- China
- Prior art keywords
- sample
- separation
- connector
- valve
- access
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000926 separation method Methods 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 230000005526 G1 to G0 transition Effects 0.000 claims description 24
- 238000002347 injection Methods 0.000 claims description 22
- 239000007924 injection Substances 0.000 claims description 22
- 230000002411 adverse Effects 0.000 claims description 14
- 239000012530 fluid Substances 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 4
- 238000004587 chromatography analysis Methods 0.000 claims description 2
- 230000008676 import Effects 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 4
- 238000010586 diagram Methods 0.000 description 10
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000004460 liquid liquid chromatography Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/38—Flow patterns
- G01N30/42—Flow patterns using counter-current
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/065—Preparation using different phases to separate parts of sample
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The present invention relates to a kind of high-speed counter-current chromatographs and method of work for complex sample multi-cycle separation, including detaching access, separation access end is connected with multiple six-way valves and circulating valve component in turn, the circulating valve component is with detaching the connection of access head end, form multi-cycle separation circuit, the circulating valve component is also associated with solvent bottle and transfer tube, the transfer tube provides power for flowing of the sample in multi-cycle separation circuit, collecting pipe is set on the multiple six-way valve, it will be in the collecting pipe access multi-cycle separation circuit of different six-way valves, realize the multi-cycle separation of multiple complex samples, the high-speed counter-current chromatograph of the present invention can realize the multi-cycle separation of sample, and it can realize the multi-cycle separation of multicomponent complex sample, good separating effect.
Description
Technical field
The present invention relates to separation equipment technical fields, and in particular to a kind of high-speed counter-current for complex sample multi-cycle separation
Chromatograph and method of work.
Background technology
High speed adverse current chromatogram is a kind of liquid-liquid chromatography isolation technics, its stationary phase and mobile phase is all liquid, without not
Reversible adsorption has many advantages, such as that sample nondestructive loses, pollution-free, efficient, quick and big preparation two detaches, for one-dimensional adverse current chromatogram
It is difficult to the sample detached, it usually needs carry out secondary separation, during secondary separation, sample is picked out by pipeline, and it is inverse to be connected to two dimension
Flow chromatography or liquid carry out secondary separation after rebalancing, and the instrument quantity needed is more, and operating process is complicated, and
For the inferior separating effect of multicomponent complex sample.
Invention content
In order to overcome above-mentioned technological deficiency, the present invention provides a kind of high-speed counter-current colors for complex sample multi-cycle separation
Spectrometer can realize the multi-cycle separation of multicomponent complex sample, and to achieve these goals, the present invention uses following technical side
Case:
A kind of high-speed counter-current chromatograph for complex sample multi-cycle separation, including detaching access, the separation access end
End is connected with multiple six-way valves and circulating valve component in turn, and the circulating valve component is connected with detaching the head end of access, and composition is followed
Ring separating circuit, the circulating valve component are connected with transfer tube between access with detaching, and the circulating valve component is fixed with containing
The solvent bottle connection of phase, transfer tube can drive stationary phase to enter separation access through circulating valve component, in the multiple six-way valve with
Separating circuit connection is head end six-way valve, and it is end six-way valve to be connect with circulating valve component, every in the multiple six-way valve
Collecting pipe is set between two connectors of a six-way valve, and two connectors of disconnected collecting pipe are as sample inlet and sample
It exports, connecting tube is set between remaining two connectors, by the collecting pipe access multi-cycle separation circuit of different six-way valves, can connect
Different cycle peaks is received, realizes the separation of complex sample.
Further, the circulating valve component is cycle six-way valve, and two connectors of the cycle six-way valve are as sample
Product import and sample export, a connector are connected with for containing the solvent bottle of stationary phase, and a connector passes through transfer tube
Connection detaches access, and connecting tube is set between remaining two connectors.
Further, the head end six-way valve is connected as the connector of sample inlet with detaching access, end six-way valve
Connector as sample export is connect with circulating valve component.
A kind of high-speed counter-current chromatograph for complex sample multi-cycle separation, including detaching access, the separation access end
End is connected with the first triple valve, multiple six-way valves and circulating valve component, head end of the circulating valve component with detaching access in turn
Connection, forms multi-cycle separation circuit, and the circulating valve component is connected with transfer tube, the circulating valve component between access with detaching
It is connected with the solvent bottle for containing stationary phase, transfer tube can drive stationary phase to enter separation access through circulating valve component, the multiple
It is head end six-way valve to be connect in six-way valve with the first triple valve, and it is end six-way valve to be connect with circulating valve component, described more
Collecting pipe is set between two connectors of a six-way valve, and two connectors of disconnected collecting pipe are as sample inlet and sample
It exports, connecting tube is set between remaining two connectors, by the collecting pipe access multi-cycle separation circuit of different six-way valves, can connect
Different cycle peaks is received, realizes the separation of complicated Multi-example.
Further, the head end six-way valve connects as the connector of sample inlet and a connector of the first triple valve
It connects, a connector of the first triple valve is with detaching access connection, and a connector of the first triple valve is as sample collection mouth.
Further, the circulating valve component is the second triple valve, a connector of second triple valve and end
Six-way valve is connected as the connector of sample export, the connector connection solvent bottle of second triple valve, a connection
Mouth connects six-way injection valve by transfer tube.
Further, the separation access includes sequentially connected six-way injection valve, current chromatographic column and detector, described
Six-way injection valve enters separation access for sample, and current chromatographic column detaches sample, and detector is used to carry out sample
Detection.
The invention also discloses a kind of method of work of the high-speed counter-current chromatograph for complex sample multi-cycle separation, including
Following steps:
Step 1:Multiple six-way valves are switched to the connector connecting with collecting pipe as the connector of sample inlet to connect
State, connect transfer tube with the connector as sample inlet of head end six-way valve, under the action of transfer tube, be pumped into stream
Dynamic phase, mobile phase flow successively through multiple six-way valves, and in end, six-way valve is flowed out as the connector of sample export, is filled in collecting pipe
Full mobile phase.
Step 2:The connector that multiple six-way valves are switched to as sample inlet connects with the connector as sample export
Logical state, transfer tube is connect with six-way injection valve and circulating valve component, under the action of transfer tube, the stationary phase in solvent bottle
Entire multi-cycle separation circuit is flowed into, finally fills entire multi-cycle separation circuit.
Step 3:Start current chromatographic column rotation, transfer tube driving stationary phase flows into multi-cycle separation circuit, until reaching stream
Body dynamics balance.
Step 4:After reaching fluid dynamic equilibrium, sample injects six-way injection valve after stationary phase and flowing phased soln,
Carry out adverse current chromatogram separation.
Further, in the step 4, for the high sample of separating degree, the sample of detector outflow is directly collected,
Realize the adverse current chromatogram separation of sample.
Further, in the step 4, the sample detached is difficult to for an adverse current chromatogram, adjusts circulating valve component, inspection
The sample of survey device outflow is again introduced into current chromatographic column through circulating valve component and is detached, and realizes the multi-cycle separation of sample, detaches
Situation is detected in real time using detector, after the completion of separation, adjusts circulating valve component, solvent bottle is made to pass through circulating valve component and driving
Pump is connect with six-way injection valve, facilitates next use.
Further, in the step 4, the separation for multicomponent complex sample connects the collecting pipe of different six-way valves
Enter in multi-cycle separation circuit, different cycle peaks can be received, realize the multi-cycle separation of complex sample, separation situation utilizes detector
Detection in real time after the completion of separation, adjusts circulating valve component, solvent bottle is made to pass through circulating valve component and transfer tube and six-way injection valve
Connection, facilitates next use.
Beneficial effects of the present invention:
1. the high-speed counter-current chromatograph of the present invention has circulating valve component, it can be achieved that the multi-cycle separation of sample, separating effect
It is good.
2. the present invention high-speed counter-current chromatograph, separated sample can quickly be collected.
3. the high-speed counter-current chromatograph of the present invention, collecting pipe is provided on six-way valve, the collecting pipe of different six-way valves accesses
In multi-cycle separation circuit, different cycle peaks can be received, realizes the separation and collection of complex sample.
Description of the drawings
The accompanying drawings which form a part of this application are used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation do not form the restriction to the application for explaining the application.
Fig. 1 is 1 solvent balance schematic diagram of the embodiment of the present invention;
Fig. 2 is 1 adverse current chromatogram separation schematic diagrames of the embodiment of the present invention;
Fig. 3 is 1 multi-cycle separation schematic diagram of the embodiment of the present invention;
Fig. 4 is 1 multimodal multi-cycle separation schematic diagram one of the embodiment of the present invention;
Fig. 5 is 1 multimodal multi-cycle separation schematic diagram two of the embodiment of the present invention;
Fig. 6 is 2 solvent balance schematic diagram of the embodiment of the present invention;
Fig. 7 is 2 adverse current chromatogram separation schematic diagrames of the embodiment of the present invention;
Fig. 8 is 2 multi-cycle separation schematic diagram of the embodiment of the present invention;
Fig. 9 is 2 multimodal multi-cycle separation schematic diagram one of the embodiment of the present invention;
Figure 10 is 2 multimodal multi-cycle separation schematic diagram two of the embodiment of the present invention;
Wherein:1. six-way injection valve, 2. current chromatographic columns, 3. detectors, 4. first six-way valves, 5. second six-way valves, 6.
Third six-way valve, 7. solvent bottles, 8. transfer tubes, 9. collecting pipes, 10. connecting tubes, 11. first triple valves, 12. second triple valves.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.It is unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
As background technology is introduced, existing high-speed counter-current chromatograph can not realize the multi-cycle separation of sample, and
For the inferior separating effect of multicomponent complex sample, in view of the above-mentioned problems, being recycled present applicant proposes one kind for complex sample
The high-speed counter-current chromatograph of separation.
In a kind of exemplary embodiments 1 of the application, a kind of high-speed counter-current chromatograph for complex sample multi-cycle separation, packet
Include separation access, the separation access includes sequentially connected six-way injection valve 1, current chromatographic column 2 and detector 3, described point
The first six-way valve 4, the second six-way valve 5 and third six-way valve 6 are connected in turn from access end, and the third six-way valve is used as and follows
Ring valve component is connected with the head end for detaching access, forms multi-cycle separation circuit, and the third six-way valve connects with detaching between access
Transfer tube is connected to, the third six-way valve is connected with containing the solvent bottle 7 of stationary phase, and transfer tube 8 can drive stationary phase through third
Six-way valve enters separation access.
Collecting pipe 9 between first six-way valve and the connector IV of the second six-way valve and connector V is set, is passed through
By in the collecting pipe of the first six-way valve or the second six-way valve access multi-cycle separation circuit, realize and receive different cycle peaks, and then
Realize the separation of multiple complex samples, the connector VI of the first six-way valve and the second six-way valve as sample inlet, make by connector I
For sample export, connecting tube 10 is set between connector II and connector III.
The connector VI of first six-way valve is connect with the outlet of detector, the connection of I and second six-way valve of connector
Mouth VI connects, and the connector I of the second six-way valve is connect with third six-way valve.
The connector IV of the third six-way valve is connected as sample inlet with the connector I of the second six-way valve, and the three or six
Connecting tube is set between the connector II of port valve and connector III, and connector I is used as sample collection mouth, and connector VI is solid with containing
Determine the solvent bottle connection of phase, connector V is connect by transfer tube with six-way injection valve.
The specific works method of embodiment 1 includes the following steps:
Step 1:Switch the first six-way valve and the second six-way valve, make the connector VI of the first six-way valve and the second six-way valve with
Connector V connects (connection status that the first six-way valve and the second six-way valve are VI → V → IV → III → II → I), will drive
Dynamic pump is connect with the connector VI of the first six-way valve with transfer tube, and transfer tube driving mobile phase enters the first six-way valve and the two or six
Port valve is finally flowed out from the connector I of the second six-way valve, at this time full of stream in the collecting pipe of the first six-way valve and the second six-way valve
Dynamic phase.
Step 2:As shown in Figure 1, the first six-way valve of switching and the second six-way valve, make its connector VI be connected with connector I,
Transfer tube is accessed between the connector V of six-way injection valve and third six-way valve, starts transfer tube, the stationary phase in solvent bottle into
Enter multi-cycle separation circuit, sequence of flow is:
Third six-way valve (VI → V)-pump-six-way injection valve-current chromatographic column-detector -- the first six-way valve (VI → I)-
Second six-way valve (VI → I)-third six-way valve
Stationary phase is flowed out by the connector I of third six-way valve, and finally, stationary phase fills entire multi-cycle separation circuit.
Step 3:Start current chromatographic column rotation, according to the sequence of step 2, stationary phase is pumped into certain flow rate, until reaching
To fluid dynamic equilibrium.
Step 4:After reaching fluid dynamic equilibrium, sample through suitable stationary phase and flowing phased soln after injection six lead into
The sample introduction circle of sample valve, sample introduction finish, and carry out adverse current chromatogram separation.
In the step 4, as shown in Fig. 2, for the high sample of separating degree, it is direct at the connector I of third six-way valve
Sample is collected, realizes the adverse current chromatogram separation of sample.
In the step 4, as shown in figure 3, being difficult to the sample detached for an adverse current chromatogram, third six-way valve is switched
The state connected to connector IV with connector V, the sample of detector outflow is through the first six-way valve, the second six-way valve, the three or six
Current chromatographic column is again introduced into after port valve and six-way injection valve, multi-cycle separation is realized, monitors separation situation in real time using detector,
Switch third six-way valve to original position, the collection of sample is carried out by connector I, sequence of flow is:
Third six-way valve (IV → V)-pump-six-way injection valve-the-the first six-way valve of current chromatographic column-detector (VI → I)-
Second six-way valve (VI → I)-third six-way valve.
When the complex sample for having multiple ingredients needs to carry out multi-cycle separation, by the receipts of the first six-way valve or the second six-way valve
In collector access circulation loop, specifically:
As shown in figure 4, the first six-way valve of switching is connected to connector VI with connector V, by the collecting pipe of the first six-way valve
It accesses in multi-cycle separation circuit, cycle peak one can be received, circulation sequence is:
Third six-way valve (IV → V)-pump-six-way injection valve-the-the first six-way valve of current chromatographic column-detector (VI → V →
IV → III → II → I) the-the second six-way valve (VI → I)-third six-way valve
As shown in figure 5, the second six-way valve of switching is connected to connector VI with connector V, by the collecting pipe of the second six-way valve
It accesses in multi-cycle separation circuit, cycle peak two can be received, circulation sequence is:
Third six-way valve (IV → V)-pump-six-way injection valve-the-the first six-way valve of current chromatographic column-detector (VI → I)-
Second six-way valve (VI → V → IV → III → II → I)-third six-way valve
Monitor separation situation in real time using detector, switching third six-way valve to original position is connected through mouth I and carries out sample
Collection.
Because sample composition to be collected can not necessarily be completely filled with collecting pipe, when switching over separation, bubble meeting
Into adverse current chromatogram, so as to influence to detach, so being pre-filled with mobile phase in collecting pipe, elimination bubble ensure that.
In another embodiment 2 of the application, be improved on the basis of embodiment 1, as illustrated in figures 6-10, detector with
The first triple valve 11 is connected between first six-way valve, detector outlet is connect with the connector II of the first triple valve, the first threeway
The connector I of valve is connect with the connector VI of the first six-way valve, and the connector III of the first triple valve is used as sample collection mouth.It is described
Circulating valve component uses the second triple valve 12, and the connector III of second triple valve is connect with the connector I of the second six-way valve,
The connector II of second triple valve is connect by transfer tube with six-way injection valve, and the connection of connector I of the second triple valve contains admittedly
Determine the solvent bottle of phase.Remaining structure is same as Example 1.
In the method for work of embodiment 2, when injecting stationary phase to fluid dynamic equilibrium, the first triple valve of switching to connection
Mouthful II with III connected state of connector, during an adverse current chromatogram separation, the first triple valve switches to connector II and connector III
Connected state carries out sample collection using the connector III of the first triple valve, and when carrying out multi-cycle separation, the first triple valve of switching is extremely
Connector II and I connected state of connector, the second triple valve of switching are recycled to connector III and II connected state of connector
Separation, the second triple valve of switching facilitates next use to connector II and I connected state of connector after the completion of separation, more when having
When a sample carries out multi-cycle separation, the operating method of the first six-way valve and the second six-way valve is same as Example 1, remaining operating method
It is same as Example 1.
Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not protects model to the present invention
The limitation enclosed, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not
Need to make the creative labor the various modifications or changes that can be made still within protection scope of the present invention.
Claims (10)
1. a kind of high-speed counter-current chromatograph for Multi-example multi-cycle separation, which is characterized in that including detaching access, the separation
Access end is connected with multiple six-way valves and circulating valve component in turn, and the circulating valve component is connected with detaching the head end of access,
Form multi-cycle separation circuit, the circulating valve component is connected with transfer tube between access with detaching, and the circulating valve component is with containing
The solvent bottle connection of stationary phase is filled, transfer tube can drive stationary phase to enter separation access through circulating valve component, and the multiple six is logical
It is head end six-way valve to be connect in valve with separating circuit, and it is end six-way valve to be connect with circulating valve component, and the multiple six is logical
Collecting pipe is set in valve between two connectors of each six-way valve, and two connectors of disconnected collecting pipe are as sample inlet
And sample export, connecting tube is set between remaining two connectors, by the collecting pipe access multi-cycle separation circuit of different six-way valves
In, different cycle peaks can be received, realizes the separation of multicomponent complex sample.
A kind of 2. high-speed counter-current chromatograph for complex sample multi-cycle separation as described in claim 1, which is characterized in that institute
Circulating valve component is stated as cycle six-way valve, two connectors of the cycle six-way valve are as sample inlet and sample export, and one
A connector is connected with for containing the solvent bottle of stationary phase, and a connector connects separation access, residue two by transfer tube
Connecting tube is set between a connector.
A kind of 3. high-speed counter-current chromatograph for complex sample multi-cycle separation as described in claim 1, which is characterized in that institute
Head end six-way valve is stated as the connector of sample inlet with detaching access connection, connector of the end six-way valve as sample export
It is connect with circulating valve component.
4. a kind of high-speed counter-current chromatograph for complex sample multi-cycle separation, which is characterized in that including detach access, described point
The first triple valve, multiple six-way valves and circulating valve component are connected in turn from access end, and the circulating valve component is logical with detaching
The head end connection on road, forms multi-cycle separation circuit, and the circulating valve component is connected with transfer tube between access with detaching, described to follow
Ring valve component is connected with containing the solvent bottle of stationary phase, and transfer tube can drive stationary phase to enter separation access through circulating valve component,
It is head end six-way valve to be connect in the multiple six-way valve with the first triple valve, and it is that end six is logical to be connect with circulating valve component
Valve sets collecting pipe between two connectors of the multiple six-way valve, and two connectors of disconnected collecting pipe are as sample
Import and sample export set connecting tube between remaining two connectors, the collecting pipe of different six-way valves are accessed multi-cycle separation
In circuit, different cycle peaks can be received, realizes the separation of multicomponent complex sample.
A kind of 5. high-speed counter-current chromatograph for complex sample multi-cycle separation as claimed in claim 4, which is characterized in that institute
The connector that head end six-way valve is stated as sample inlet is connect with a connector of the first triple valve, one of the first triple valve
Connector is with detaching access connection, and a connector of the first triple valve is as sample collection mouth.
A kind of 6. high-speed counter-current chromatograph for complex sample multi-cycle separation as claimed in claim 4, which is characterized in that institute
The connector that head end six-way valve is stated as sample inlet is connect with a connector of the first triple valve, one of the first triple valve
Connector is with detaching access connection, and a connector of the first triple valve is as sample collection mouth.
A kind of 7. high-speed counter-current chromatograph for complex sample multi-cycle separation as claimed in claim 4, which is characterized in that institute
Circulating valve component is stated as the second triple valve, a connector and end six-way valve for second triple valve is as sample export
Connector connects, and the connector connection solvent bottle of second triple valve a, connector is connected by transfer tube and detached
Access.
8. a kind of high-speed counter-current chromatograph for complex sample multi-cycle separation as described in claim 1 or 4, feature exist
In:The separation access includes sequentially connected six-way injection valve, current chromatographic column and detector, and the six-way injection valve is used for
Sample enters separation access, and current chromatographic column detaches sample, and detector is used to be detected sample.
9. a kind of method of work of high-speed counter-current chromatograph for complex sample multi-cycle separation as described in claim 1 or 4,
It is characterized by comprising the following steps:
Step 1:Multiple six-way valves are switched to the shape that the connector being connect as the connector of sample inlet with collecting pipe connects
State is connect transfer tube with the connector as sample inlet of head end six-way valve, under the action of transfer tube, is pumped into flowing
Phase, mobile phase flow successively through multiple six-way valves, and in end, six-way valve is flowed out as the connector of sample export, is full of in collecting pipe
Mobile phase.
Step 2:What the connector that multiple six-way valves are switched to as sample inlet was connected with the connector as sample export
State, transfer tube is connect with six-way injection valve and circulating valve component, and under the action of transfer tube, the stationary phase in solvent bottle flows into
Entire multi-cycle separation circuit, finally fills entire multi-cycle separation circuit.
Step 3:Start current chromatographic column rotation, transfer tube driving stationary phase flows into multi-cycle separation circuit, moved until reaching fluid
Mechanical balance.
Step 4:After reaching fluid dynamic equilibrium, sample injection separation access after stationary phase and flowing phased soln carries out inverse
Flow chromatography detaches.
10. a kind of method of work of high-speed counter-current chromatograph for Multi-example multi-cycle separation as claimed in claim 9, special
Sign is, in the step 4, for the high sample of separating degree, the sample of separation access outflow is directly collected, and realizes sample
An adverse current chromatogram separation;
In the step 4, the sample detached is difficult to for an adverse current chromatogram, adjusts circulating valve component, the sample of detector outflow
Product are again introduced into separation access through circulating valve component and are detached, and realize the multi-cycle separation of sample, and separation situation monitors in real time, point
From after the completion, circulating valve component is adjusted, solvent bottle is made to pass through circulating valve component and transfer tube with detaching access connection, facilitates next time
It uses;
In the step 4, the separation for multicomponent complex sample, by the collecting pipe access multi-cycle separation circuit of different six-way valves
In, different cycle peaks can be received, realizes the multi-cycle separation of complex sample, separation situation monitors in real time, after the completion of separation, adjustment
Circulating valve component makes solvent bottle pass through circulating valve component and transfer tube with detaching access connection, facilitates next use.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810194444.1A CN108254475A (en) | 2018-03-09 | 2018-03-09 | A kind of high-speed counter-current chromatograph and method of work for complex sample multi-cycle separation |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810194444.1A CN108254475A (en) | 2018-03-09 | 2018-03-09 | A kind of high-speed counter-current chromatograph and method of work for complex sample multi-cycle separation |
Publications (1)
Publication Number | Publication Date |
---|---|
CN108254475A true CN108254475A (en) | 2018-07-06 |
Family
ID=62745927
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810194444.1A Pending CN108254475A (en) | 2018-03-09 | 2018-03-09 | A kind of high-speed counter-current chromatograph and method of work for complex sample multi-cycle separation |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108254475A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113149813A (en) * | 2021-04-20 | 2021-07-23 | 金溪华香香料有限公司 | Linalool purification and separation device based on high-speed countercurrent chromatographic separation |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5630943A (en) * | 1995-11-30 | 1997-05-20 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Discontinuous countercurrent chromatographic process and apparatus |
CN101637665A (en) * | 2009-01-09 | 2010-02-03 | 中山大学 | Method for combined use of accelerated solvent extraction and high speed countercurrent chromatogram and device thereof |
CN104267131A (en) * | 2014-09-30 | 2015-01-07 | 浙江工业大学 | Ion chromatography single pump-column switching system for detecting trace inorganic anions in weak-acid salt |
CN104645667A (en) * | 2013-11-18 | 2015-05-27 | 华东理工大学 | Expanded bed chromatography and counter-current chromatography on-line combination method, application and apparatus thereof |
CN206038625U (en) * | 2016-09-09 | 2017-03-22 | 中国科学院西北高原生物研究所 | General type high -speed countercurrent chromatograph circulates |
CN107151203A (en) * | 2016-03-03 | 2017-09-12 | 复旦大学 | Separate the method for preparing natural naphthoquinone compound |
CN107652260A (en) * | 2016-07-24 | 2018-02-02 | 复旦大学 | The method that high speed adverse current chromatogram quick separating prepares natural flavanone kind composition |
-
2018
- 2018-03-09 CN CN201810194444.1A patent/CN108254475A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5630943A (en) * | 1995-11-30 | 1997-05-20 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Discontinuous countercurrent chromatographic process and apparatus |
CN101637665A (en) * | 2009-01-09 | 2010-02-03 | 中山大学 | Method for combined use of accelerated solvent extraction and high speed countercurrent chromatogram and device thereof |
CN104645667A (en) * | 2013-11-18 | 2015-05-27 | 华东理工大学 | Expanded bed chromatography and counter-current chromatography on-line combination method, application and apparatus thereof |
CN104267131A (en) * | 2014-09-30 | 2015-01-07 | 浙江工业大学 | Ion chromatography single pump-column switching system for detecting trace inorganic anions in weak-acid salt |
CN107151203A (en) * | 2016-03-03 | 2017-09-12 | 复旦大学 | Separate the method for preparing natural naphthoquinone compound |
CN107652260A (en) * | 2016-07-24 | 2018-02-02 | 复旦大学 | The method that high speed adverse current chromatogram quick separating prepares natural flavanone kind composition |
CN206038625U (en) * | 2016-09-09 | 2017-03-22 | 中国科学院西北高原生物研究所 | General type high -speed countercurrent chromatograph circulates |
Non-Patent Citations (1)
Title |
---|
谭志斗 等: "现代化学分离技术原理及研究进展", 中国原子能出版社, pages: 177 - 180 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113149813A (en) * | 2021-04-20 | 2021-07-23 | 金溪华香香料有限公司 | Linalool purification and separation device based on high-speed countercurrent chromatographic separation |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN104713973B (en) | There is two-dimentional preparative hplc instrument system and the application thereof of on-line preconcentration function | |
CN107121504B (en) | Multi-functional temperature-pressure extraction-trapping-chromatographic isolation on-line coupling equipment | |
CN102580352B (en) | Separation method of natural product | |
CN207586196U (en) | The multidimensional liquid chromatographic separation system of full on-line checking based on same detector | |
CN105606753B (en) | Field auxiliary extraction-separation and concentration-chromatography on-line coupling equipment | |
CN102961892A (en) | Preparative multidimensional liquid chromatographic instrument | |
CN102590396B (en) | Two-dimensional liquid chromatography device | |
CN108490107A (en) | A kind of liquid chromatograph and working method for complex sample multi-cycle separation | |
CN101791491B (en) | Online low-pressure, middle-pressure and high-pressure combined two-dimension preparation liquid chromatographic system | |
CN110208401A (en) | Solid phase is dehydrated extraction-supercritical fluid chromatography-mass spectrum on-line analysis system and method | |
CN104606921A (en) | Double-column cyclic preparation HPLC (high performance liquid chromatograph) and method for preparation, separation and purification | |
CN204989098U (en) | Capillary electrophoresis and electrochromatography plug -in components | |
CN207198107U (en) | A kind of cascade Coupled columns mass spectrometer system based on valve | |
CN108254475A (en) | A kind of high-speed counter-current chromatograph and method of work for complex sample multi-cycle separation | |
CN104614458A (en) | Recycling preparative HPLC (high performance liquid chromatograph) provided with multi-ported valve | |
CN207851002U (en) | Multidimensional counter-current chromatograph for complex sample multi-cycle separation | |
CN205844281U (en) | What a kind of bidimensional analysis was carried out simultaneously arrheas type two-dimensional liquid chromatography | |
CN207908445U (en) | A kind of high-speed counter-current chromatograph for complex sample multi-cycle separation | |
CN201348625Y (en) | Multidimensional chromatography separator | |
CN108226358A (en) | For the multidimensional counter-current chromatograph and method of work of complex sample multi-cycle separation | |
CN207816918U (en) | A kind of liquid chromatograph for complex sample multi-cycle separation | |
CN113341030B (en) | High-flux liquid chromatography-mass spectrometry system and separation and analysis method | |
CN106053668B (en) | What bidimensional analysis was carried out at the same time arrheas type two-dimensional liquid chromatography and its application | |
CN104645667B (en) | Expanded bed chromatography and counter-current chromatography on-line combination method, application and apparatus thereof | |
CN217060099U (en) | Multi-mode liquid chromatography system |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180706 |