CN109557219A - A kind of multidimensional liquid chromatographic separation system - Google Patents
A kind of multidimensional liquid chromatographic separation system Download PDFInfo
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- 238000013375 chromatographic separation Methods 0.000 title claims abstract description 26
- 238000000926 separation method Methods 0.000 claims abstract description 79
- 238000005070 sampling Methods 0.000 claims abstract description 30
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 27
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 24
- 238000007865 diluting Methods 0.000 claims abstract description 18
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 18
- 239000007791 liquid phase Substances 0.000 claims abstract description 8
- 238000007445 Chromatographic isolation Methods 0.000 claims abstract description 6
- 238000000105 evaporative light scattering detection Methods 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims 4
- 238000010828 elution Methods 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 5
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- 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
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- 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
- G01N30/08—Preparation using an enricher
-
- 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
- G01N30/60—Construction of the column
- G01N30/6034—Construction of the column joining multiple columns
- G01N30/6043—Construction of the column joining multiple columns in parallel
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Abstract
The present invention provides a kind of multidimensional liquid chromatographic separation system, including high performance liquid chromatography gradient pump A, high performance liquid chromatography gradient pump B, efficient liquid phase diluting pump, gradient mixer A, gradient mixer B, sampling valve, enriching column array A, enriching column array B, fraction collector, liquid chromatography separation column array, detector, two ten-way valves and connecting line；The three-dimensional or three-dimensional above chromatographic isolation is realized in the conversion that upper one-dimensional discrete state one-dimensional discrete state under is realized by two ten-way valve switchings.Each dimension chromatography column is selected by liquid chromatography separation column array, is based on same gradient elution system and same detector, full on-line monitoring and the control of multi-dimensional chromatograph separation is realized, realizes that enriching column and splitter clean-up performance are controllable.Each dimension separation is connected by enriching column, and is enriched with or is trapped using diluting pump auxiliary compounds.The present invention is by selecting different chromatographic stationary phases and flowing to be combined, and monomeric compound efficiently separates in the realization complex system sample high to separating difficulty.
Description
Technical field
The invention belongs to high performance liquid chromatography separation technical fields, are related to a kind of multidimensional liquid chromatographic separation system.
Background technique
With the development of isolation technics, seeks and separate the ingredient in complex sample system and have become hot research field.
The separating degree that Multidimensional Liquid Chromatography Technology is effectively improved the separation of complex sample ingredient by improving peak capacity, becomes flash chromatography point
From technological development direction.Multidimensional Liquid Chromatography Technology is that the eluent of the first dimension chromatographic column of sample is implanted sequentially subsequent dimension
The liquid chromatogram joint technology that chromatographic column is further separated.This isolation technics can use two or more difference
The chromatographic column of separating mechanism carries out the orthogonal separation of sample.The most common multidimensional liquid chromatogram interfacing has 3 kinds: being based on sample
The interfacing of ring；Interfacing based on enriching column (also referred to as trapping column)；Interfacing based on dwell pattern.
Currently, multidimensional liquid chromatographic separation system mainly includes arrheaing type two-dimensional liquid chromatography system, continuous loop switch type
Two-dimensional liquid chromatography system and serial mode multidimensional liquid chromatographic system.
Arrhea type two-dimensional liquid chromatography system running pattern are as follows: the first dimension separation system stops after separating one section of sample, point
Sample from after is transferred to the second dimension separation system and is separated, and stops after the completion of the second dimension separation system, continues the first dimension point
Operation from system, moves in circles, and completes all separation.
Continuous loop switch type two-dimensional liquid chromatography system running pattern are as follows: one section of sample of the first dimension separation system separation is handed over
It is separated to the second dimension separation system, the first dimension separation system continues the separation of the first dimension, and so on, completes all points
From.Continuous loop switch type two-dimensional liquid chromatography system separating rate is exceedingly fast, but the separation of two-dimensional liquid chromatography is by the first dimension
Liquid chromatogram seriously restricts, and application field receives certain restrictions.
Serial mode multidimensional liquid chromatographic system operational mode are as follows: the first dimension separation system is first run, by the sample after separation
Successively accurately cutting is enriched in multiple enriching columns product component, after the first dimension separation, then starts two dimensional separation；It is so past
It is multiple, realize multi-dimensional chromatograph separation.Serial mode multidimensional liquid chromatographic system is with the full-automatic height of German Sepiatec GmbH company
Flux preparative separation system sepbox series of products are representative, but the product can only carry out Two way chromatograms separation, separating capacity
It is limited.
Chinese patent application CN108037233A discloses a kind of multidimensional liquid of full on-line checking based on same detector
Phase chromatographic fractionation system realizes that separation process whole process is measurable and controllable, and enriching column and splitter clean-up performance can detecte, and be suitable for
Highly difficult replicate analysis, separation and the preparation of complex sample system are easy to implement the efficient preparation of monomeric compound.The system category
In serial mode multidimensional liquid chromatographic system.But the entrance and exit of the system enriching column array be it is fixed, work as enriching column
When as loading column, the flow direction of eluent is consistent with the flow direction of mobile phase when enriched sample originally, and sample one
As be enriched in the entrance of enriching column, it is therefore desirable to more mobile phase and more time could complete the upper of sample in enriching column
Sample.
Summary of the invention
The purpose of the present invention is taking a long time for existing multidimensional liquid chromatographic separation system, mobile phase consumes biggish spy
Point reduces the separation of multidimensional liquid chromatographic separation system on the basis of retaining existing multidimensional liquid chromatographic separation system advantage
The consumption of time and mobile phase.
In order to achieve the above object, the technical solution of the present invention is as follows:
A kind of multidimensional liquid chromatographic separation system, including high performance liquid chromatography gradient pump A, high performance liquid chromatography gradient pump B,
Diluting pump, gradient mixer A, gradient mixer B, sampling valve, enriching column array A, enriching column array B, fraction collector, liquid
Phase chromatography column array, detector, two ten-way valves and connecting line.The 1. position of two ten-way valves, 2. position, 3.
Position, 4. position, 5. position, 6. position, 7. position, 8. position, 9. position, 10. position only indicates syntople, it is not necessary to the physics mark with two ten-way valves
Note corresponds to, and the name of number position and is ordered as since any interface of two ten-way valves according to counterclockwise or clockwise since 1.
Sequence name.The detector is used to detect the chromatographic signal in separation process.
The liquid chromatography separation column array is to be formed in parallel by multiple chromatography columns by multidigit selector valve, same
Moment can only have a chromatography column conducting；Externally there are a fixed entrance and a fixed outlet, and at least one
A bypass, the bypass and splitter are in parallel by multidigit selector valve；When by-path turn-on, other chromatography columns cannot be connected,
When the conducting of other chromatography columns, bypass cannot be connected；Depending on the quantity of chromatography column is as needed, if it is three-dimensional,
Then it is recommended as 3 splitters, if it is the four-dimension, is then recommended as 4 splitters.
The enriching column array A, enriching column array B are formed in parallel by multiple chromatograph enrichment columns by multidigit selector valve,
There can only be an enriching column conducting in synchronization；At least one bypass, the bypass and enriching column pass through multidigit selector valve simultaneously
Connection；When by-path turn-on, other enriching columns cannot be connected, and when the conducting of other enriching columns, bypass cannot be connected；Externally have two
A interface is respectively defined as interface X and interface Y；Depending on the quantity of enriching column is as needed, it is primarily limited to length of pipe and peace
Fill space.Multiple enriching column arrays can connect, i.e. the interface of the interface Y of upper level enriching column array and secondary enriching column array
X connection constitutes multistage enriching column array, and operation control is consistent with single-stage enriching column array, and synchronization can only have an enrichment
Column conducting；When the multistage enriching column array is by-path turn-on state then every grade of enriching column array all in by-path turn-on.
The high performance liquid chromatography gradient pump A and high performance liquid chromatography gradient pump B are connect with the entrance of gradient mixer A,
The outlet of gradient mixer A is connect with sampling valve, and the outlet of sampling valve is connect with a 1. number position for two ten-way valves；Two ten-way valves
10. number position connect with the interface X of enriching column array A, the interface Y of enriching column array A is connect with a 7. number position for two ten-way valves；
The 6. number position of two ten-way valves is connect with the entrance of liquid chromatography separation column array, the outlet and inspection of liquid chromatography separation column array
Device connection is surveyed, the outlet of detector is connect with the entrance of gradient mixer B, and diluting pump is connect with the entrance of gradient mixer B,
The outlet of gradient mixer B is connect with a 8. number position for two ten-way valves；The 9. number position of two ten-way valves is connect with a 4. number position；Two
The 5. number position of ten-way valve is connect with the Y interface of enriching column array B, the 2. number position of the X interface of enriching column array B and two ten-way valves
Connection；The 3. entrance of number position and fraction collector connection of two ten-way valves.
Based on the pipeline connecting mode of above-mentioned multidimensional liquid chromatographic separation system, by the switching shape for controlling two ten-way valves
State, realization system are converted to down one-dimensional discrete state from upper one-dimensional discrete state, complete cyclical chromatography function, realize that multidimensional exists entirely
The chromatographic isolation function of line detection.
Sampling valve described in above-mentioned multidimensional liquid chromatographic separation system can also be connected to enriching column array A or enriching column
In the bypass of array B；At this point, the outlet of gradient mixer A is connect with a 1. number position for two ten-way valves；Above-mentioned connection changes not shadow
The use of acoustic system only redefines the dimension of enriching column in control.
Two ten-way valves can be a valve, can also be switched by one or more valve groups at and by two ten-way valves
The operation of valve principle.The sampling valve is a sampling device, can be two six logical switch sampling valves or sample injector；It can
Multidigit to be other realization liquid or solid-state loading switches loading valve；It is also possible to the chromatographic column of a realization solid-state loading.
The high performance liquid chromatography gradient pump A, high performance liquid chromatography gradient pump B are made of two modular pumps, or by one
A polynary gradient pump composition.The diluting pump is efficient liquid phase diluting pump, is a modular pump, or is a polynary pump.
The high performance liquid chromatography gradient pump A and high performance liquid chromatography gradient pump B and diluting pump, diluent can for water, salting liquid,
Methanol, acetonitrile, acetone, ethyl alcohol or normal alkane solvent, eluant, eluent can be methanol, acetonitrile, ethyl alcohol, water and its mixture, just
The common organic solvent such as structure alkane.
The detector is various for detecting the device of chromatographic signal in separation process, includes but are not limited to ultraviolet inspection
Device, diode array detector, evaporative light scattering detector or mass detector are surveyed, can be one or more detector connection
It closes.
The splitter array, enriching column array A, enriching column array B chromatographic column can select identical or different fill out
Material, the filler can be silica gel, and reverse phase silica gel matrix fill or various macropores with C18, Xion, C8, CN base or amino are inhaled
The fillers such as attached resin and ion exchange resin.
Multi-position switching valve is a kind of way of realization of column array；It should when there is a pillar conducting in a column array column
Other pillars and bypass will be not turned in column array, and when column array bypass conducting, other pillars are not turned in the column array.
The advantages of present invention preserves existing Multidimensional Liquid Chromatography Technologies, compared with existing Multidimensional Liquid Chromatography Technology, this
The innovative point and beneficial effect of invention are:
The entrance and exit of enriching column array be not it is fixed, when enriching column is as loading column, the flowing of eluent
The flow direction of direction and mobile phase when enriched sample originally on the contrary, and sample is generally enriched in the entrance of enriching column, because
This needs little flow phase and less time that can complete the elution and loading of sample in enriching column, so reduce total score from when
Between, improve separative efficiency.
Detailed description of the invention
Fig. 1 is that the odd numbers such as the first dimension of multidimensional liquid chromatographic separation system provided by the invention, the third dimension tie up discrete state
Pipeline jointing construction figure, two ten-way valves are A condition；
Fig. 2 is the Even-dimensionals discrete states such as the second dimension of multidimensional liquid chromatographic separation system provided by the invention, fourth dimension
Pipeline jointing construction figure, two ten-way valves are B state；
Fig. 3 is the pipeline jointing construction figure of liquid chromatography separation column array；
Fig. 4 is the pipeline jointing construction figure of enriching column array A, enriching column array B；
Fig. 5 (a) is two six-way injection valve sample loading condition (LOAD state, A condition) pipeline jointing construction figures, the shape
Sample is loaded into quantitative loop under state, wherein 4. number position is defined as the entrance of sampling valve, 5. number position is defined as going out for sampling valve
Mouthful；
Fig. 5 (b) is two six-way injection valve sample loading condition (INJECT state, B state) pipeline jointing construction figures, should
Sample will be separated from being injected into separation system flow path in quantitative loop under state, wherein 4. number position is defined as entering for sampling valve
Mouthful, 5. number position is defined as the outlet of sampling valve；
Fig. 6 (a) is the Multidimensional HPLC separation system structure chart of the embodiment of the present invention, and two ten-way valves are A shape
State；
In Fig. 6 (a): 1 high performance liquid chromatography gradient pump A, 2 high performance liquid chromatography gradient pump B, 3 diluting pumps, 4 gradients are mixed
Clutch A, 5 gradient mixer B, 6 sampling valves, 7 enriching column array A, 8 enriching column array B, 9 fraction collectors, 10 liquid chromatograies point
From column array, 11 detectors, 12 two ten-way valves；
Fig. 6 (b) is the Multidimensional HPLC separation system structure chart of the embodiment of the present invention, and two ten-way valves are B shape
State.
Specific embodiment
Embodiments discussed below is only a kind of description for applying to the invention patent, not to the scope of the present invention into
Row limits, and without departing from the spirit of the design of the present invention, those of ordinary skill in the art make the present invention program each
Kind modification and improvement should all fall into the protection scope that claims of the present invention determines.
A kind of multidimensional liquid chromatographic separation system, including high performance liquid chromatography gradient pump A, high performance liquid chromatography gradient pump B,
Diluting pump, gradient mixer A, gradient mixer B, sampling valve, enriching column array A, enriching column array B, fraction collector, liquid
Phase chromatography column array, detector, two ten-way valves and connecting line.Wherein, diluting pump is efficient liquid phase dilution
Pump.
The high performance liquid chromatography gradient pump A and high performance liquid chromatography gradient pump B are connect with the entrance of gradient mixer A,
The outlet of gradient mixer A is connect with sampling valve, and the outlet of sampling valve is connect with a 1. number position for two ten-way valves, two ten-way valves
10. number position connect with the X interface of enriching column array A, the Y interface of enriching column array A is connect with a 7. number position for two ten-way valves,
The 6. number position of two ten-way valves is connect with the entrance of liquid chromatography separation column array, the outlet and inspection of liquid chromatography separation column array
Device connection is surveyed, the outlet of detector is connect with the entrance of gradient mixer B, and diluting pump is connect with the entrance of gradient mixer B,
The outlet of gradient mixer B is connect with a 8. number position for two ten-way valves；The 9. number position of two ten-way valves is connect with a 4. number position；Two
The 5. number position of ten-way valve is connect with the Y interface of enriching column array B, the 2. number position of the X interface of enriching column array B and two ten-way valves
Connection；The 3. entrance of number position and fraction collector connection of two ten-way valves.The 1. position of two ten-way valves, 2. position, 3. position, 4.
Position, 5. position, 6. position, 7. position, 8. position, 9. position, 10. position only indicates syntople, it is not necessary to the physical markings pair with two ten-way valves
It answers.
Two ten-way valves are A condition in Fig. 1, at this point, high performance liquid chromatography gradient pump A and high performance liquid chromatography gradient pump B
Chromatographic isolation gradient elution mobile phase feed system is formed with gradient mixer A, the outlet of gradient mixer A and sampling valve connect
It connects, the outlet of sampling valve is connect with a 1. number position for two ten-way valves；The 1. number position of two ten-way valves be connected with a 10. number position and with richness
Interface X (the interface X of enriching column array A is its entrance at this time) connection of clustered column array A；The interface Y of enriching column array A is (at this time
The interface Y of enriching column array A exports for it) it is connect with the 7. number position of two ten-way valves and 6. number position and liquid through two ten-way valves
The entrance of phase chromatography column array connects；Any chromatographic column in selection splitter array is separated；Splitter array
Outlet is connect with detector, and detector detects chromatographic signal, and the outlet of detector is connect with the entrance of gradient mixer B, is diluted
Liquid pump is connect with the entrance of gradient mixer B, and sample, the outlet gradient mixer B and two are flowed out after gradient mixer B dilutes column
The 8. number position connection of position ten-way valve；The 8. number position of two ten-way valves is connected with a 9. number position；The 9. number position of two ten-way valves with 4. number
Position connection, the 4. number position of two ten-way valves is connected with a 5. number position；The 5. number position of two ten-way valves and the interface Y of enriching column array B
(the interface Y of enriching column array B is its entrance at this time) connection, the interface X (interface of enriching column array B at this time of enriching column array B
X exports for it) it is connect with a 2. number position for two ten-way valves, realize the enrichment of separation sample；The 3. number position of two ten-way valves with evaporate
The entrance connection of part collector, realizes sample collection.
Two ten-way valves are B state in Fig. 2, at this point, high performance liquid chromatography gradient pump A and high performance liquid chromatography gradient pump B
Chromatographic isolation gradient elution mobile phase feed system is formed with gradient mixer A, the outlet of gradient mixer A and sampling valve connect
It connects, the outlet of sampling valve is connect with a 1. number position for two ten-way valves, and the 1. number position of two ten-way valves is connected with a 2. number position；Two ten
The 2. number position of port valve connect (the interface X of enriching column array B is its entrance at this time) with the interface X of enriching column array B；Enriching column battle array
The interface Y (the interface Y of enriching column array B exports at this time for it) of column B is connect with a 5. number position for two ten-way valves；Two ten-way valves
5. number position be connected with a 6. number position, the 6. number position of two ten-way valves is connect with the entrance of liquid chromatography separation column array；Selection point
It is separated from any chromatographic column in column array；The outlet of splitter array is connect with detector, and detector detects chromatography letter
Number, the outlet of detector is connect with the entrance of gradient mixer B, and diluting pump is connect with the entrance of gradient mixer B, through gradient
Sample is flowed out after mixer B dilution column, the outlet gradient mixer B is connect with a 8. number position for two ten-way valves；Two ten-way valves
8. number position is connected with a 7. number position；The 7. position of two ten-way valves connect with the interface Y of enriching column array A (enriching column array A at this time
Interface Y is its entrance)；The interface X (the interface X of enriching column array A exports at this time for it) and two ten-way valves of enriching column array A
The connection of 10. number position, realize the enrichment of separation sample；The 10. number position of two ten-way valves is connected with a 9. number position；Two ten-way valves are 9.
Number position is connect with a 4. number position；The 4. number position of two ten-way valves is connected with a 3. number position；3. number position and the Fraction collection of two ten-way valves
The entrance of device connects, and realizes sample collection.
A kind of embodiment: Multidimensional HPLC separation system structure
Enriching column array A has 9 enriching columns in the embodiment, and number consecutively is the 1st enriching column of enriching column array A, the 2nd
Enriching column, etc., the 9th enriching column that the last one number is enriching column array A；Enriching column array B is two-stage enriching column array,
Every grade of enriching column array has 9 enriching columns, i.e. enriching column array B is 18 enriching columns, and number consecutively is the of enriching column array B
1 enriching column, the 2nd enriching column, etc., the 18th enriching column that the last one number is enriching column array B；Liquid chromatography separation column battle array
5 splitters are shown, number consecutively is the 1st splitter, and the 2nd splitter, etc., last root is the 5th splitter；In Fig. 6 (a)
Two ten-way valves be A condition, two ten-way valves in Fig. 6 (b) are B state.
The following are the four-dimensional separation process of above-mentioned Multidimensional HPLC separation system structure controls:
The operational mode of multidimensional liquid chromatographic separation system mainly includes two kinds, the first is that separation-enrichment repeatedly follows
Ring is finally terminated with separation；It is for second the multiple circulation of Rich Internet Applications, is finally also terminated with separation.It is briefly described as follows one
The four-dimensional liquid chromatogram of kind separates control process.
Enriching column and splitter are cleaned first；Successively switch each enriching column and splitter into flow path, observes detector
Signal judges cleaning effect.
First dimension separation process control: two ten-way valves are A condition, referring to Fig. 1；Enriching column array A is in bypass condition；
Quantitative loop sample being loaded on sampling valve；Selection the first dimension chromatography column, for example, the 1st splitter, the chromatography column
Conducting manually；When sampling valve is switched to INJECT state, start the first dimension separation；Under diluting pump assistance, according to sample
Property and detection signal successively by fraction using enriching column array B the 1st to the 9th enriching column in be enriched with, enriching column array B
The the 10th to the 18th enriching column give over to the third dimension separation when use；Repeatedly, until the 1st to the 9th enrichment of enriching column array B
There are enough compounds in column, is transferred to the second dimension separation process control；If you do not need to two dimensional separation, then enriching column battle array
Column B is constantly in bypass condition, and the collection of multiple fractions is directly carried out using fraction collector 9.
Second dimension separation process control: after the first dimension separation process control, sampling valve should switch to LOAD state,
Two ten-way valves switch to B state, referring to fig. 2；Selection the second dimension chromatography column, for example, the 2nd splitter, the chromatographic isolation
Column is connected manually；Select a sample of the enriching column as two dimensional separation in the 1st to the 9th enriching column of enriching column array B
Column；When enriching column conducting, the second dimension separation process starts；Under diluting pump assistance, believed according to properties of samples and detection
Number successively fraction is switched in the 1st to the 9th enriching column of enriching column array A and is enriched with；If you do not need to the third dimension separates,
Then the 1st to the 9th enriching column of enriching column array A can successively be eluted, the receipts of multiple fractions are directly carried out using fraction collector
Collection；Repeatedly, two dimensional separation is completed；
Third dimension separation process control: after the second dimension separation process control, two ten-way valves switch to A condition, ginseng
See Fig. 1；Sampling valve keeps LOAD state；Third dimension chromatography column is selected, for example, the 3rd splitter, the chromatography column is manual
Conducting；The sample column for selecting an enriching column in the 1st to the 9th enriching column of enriching column array A to separate as the third dimension；When this
When enriching column is connected, third dimension separation process starts；If necessary to carry out fourth dimension separation, then under diluting pump assistance, root
Successively fraction is switched to according to properties of samples and detection signal in the 10th to the 18th enriching column of enriching column array B and is enriched with,
It is 9 parts by faction cut；If you do not need to carry out fourth dimension separation, then can by the 1st to the 9th enriching column of enriching column array A according to
Secondary elution separation, the collection of multiple fractions is directly carried out using fraction collector；Repeatedly, third dimension separation is completed.
Fourth dimension separation process control: after third dimension separation process controls, two ten-way valves switch to B state, ginseng
See Fig. 2；Sampling valve keeps LOAD state；Fourth dimension chromatography column is selected, for example, the 4th splitter, the chromatography column is manual
Conducting；The sample column for selecting an enriching column in the 10th to the 18th enriching column of enriching column array B to separate as fourth dimension；When
When the enriching column is connected, fourth dimension separation process starts；It, can will be in the enriching column as sample column under gradient eluent effect
Compound elution, the 4th splitter effect under, carry out fourth dimension separation；Multiple fractions are received using fraction collector
Collection；Repeatedly, fourth dimension separation is completed.
Claims (10)
1. a kind of multidimensional liquid chromatographic separation system, which is characterized in that the multidimensional liquid chromatographic separation system includes efficient
Liquid chromatogram gradient pump A, high performance liquid chromatography gradient pump B, diluting pump, gradient mixer A, gradient mixer B, sampling valve,
Enriching column array A, enriching column array B, fraction collector, liquid chromatography separation column array, detector, two ten-way valves and company
Take over road；The 1. position of two ten-way valves, 2. position, 3. position, 4. position, 5. position, 6. position, 7. position, 8. position, 9. position, 10. position only table
Show syntople, it is not necessary to which corresponding with the physical markings of two ten-way valves, times from two ten-way valves is named and be ordered as in number position
Meaning interface starts according to the counterclockwise or sequence name since 1. clockwise；The detector is used to detect the color in separation process
Spectrum signal；The sampling valve is used for sample introduction；
The liquid chromatography separation column array is formed in parallel by multiple chromatography columns by multidigit selector valve, in synchronization
There can be a chromatography column conducting；To being externally provided with a fixed entrance and a fixed outlet, and by least one
Road, the bypass and splitter are in parallel by multidigit selector valve；When by-path turn-on, other chromatography columns cannot be connected, when it
Bypass cannot be connected when its chromatography column is connected；The quantity of chromatography column determines as needed；
Enriching column array A, the enriching column array B is formed in parallel by multiple chromatograph enrichment columns by multidigit selector valve,
Synchronization can only have an enriching column conducting；At least one bypass, the bypass and enriching column are in parallel by multidigit selector valve；
When by-path turn-on, other enriching columns cannot be connected, and when the conducting of other enriching columns, bypass cannot be connected；The number of enriching column
Amount determines as needed；Externally there are two interfaces, are respectively defined as interface X and interface Y；
The high performance liquid chromatography gradient pump A and high performance liquid chromatography gradient pump B are connect with the entrance of gradient mixer A, gradient
The outlet of mixer A and the entrance of sampling valve connect, and the outlet of sampling valve is connect with a 1. number position for two ten-way valves, and two ten logical
The 10. number position of valve is connect with the interface X of enriching column array A, and the 7. number position of the interface Y of enriching column array A and two ten-way valves connects
It connects, the 6. number position of two ten-way valves is connect with the entrance of liquid chromatography separation column array, the outlet of liquid chromatography separation column array
It is connect with detector, the outlet of detector is connect with the entrance of gradient mixer B, the entrance of diluting pump and gradient mixer B
Connection, the outlet of gradient mixer B is connect with a 8. number position for two ten-way valves；The 9. number position of two ten-way valves connects with 4. number position
It connects；The 5. number position of two ten-way valves is connect with the interface Y of enriching column array B, the interface X of enriching column array B and two ten-way valves
The connection of 2. number position；The 3. entrance of number position and fraction collector connection of two ten-way valves；
By controlling the switching state of two ten-way valves, realization system is converted to down one-dimensional separation shape from upper one-dimensional discrete state
State completes cyclical chromatography function, realizes the chromatographic isolation function of the full on-line checking of multidimensional.
2. a kind of multidimensional liquid chromatographic separation system according to claim 1, which is characterized in that the multidimensional liquid phase color
Sampling valve can also be connected in the bypass of enriching column array A or enriching column array B in spectrum separation system；At this point, gradient is mixed
The outlet of clutch A is connect with a 1. number position for two ten-way valves；Above-mentioned connection variation does not influence the use of system, only need to be in control
Redefine the dimension of enriching column.
3. a kind of multidimensional liquid chromatographic separation system according to claim 1 or 2, which is characterized in that the multiple enrichment
Column array can be with multistage enriching column array in series, and operation control is consistent with single-stage enriching column array, and synchronization can only have
One enriching column conducting；When the multistage enriching column array is by-path turn-on state then every grade of enriching column array all in bypass
Conducting.
4. a kind of multidimensional liquid chromatographic separation system according to claim 1 or 2, which is characterized in that described two ten logical
Valve can be a valve, can also be run by one or more valve groups at and by two ten-way valve switching valve principles.
5. a kind of multidimensional liquid chromatographic separation system according to claim 3, which is characterized in that two ten-way valves can
To be a valve, can also be run by one or more valve groups at and by two ten-way valve switching valve principles.
6. a kind of multidimensional liquid chromatographic separation system described according to claim 1 or 2 or 5, which is characterized in that described is efficient
Liquid chromatogram gradient pump A, high performance liquid chromatography gradient pump B are made of two modular pumps, or are made of a polynary gradient pump；
The diluting pump is a modular pump, or is a polynary pump.
7. a kind of multidimensional liquid chromatographic separation system according to claim 3, which is characterized in that the high-efficient liquid phase color
Spectrum gradient pump A, high performance liquid chromatography gradient pump B are made of two modular pumps, or are made of a polynary gradient pump；It is described dilute
Releasing liquid pump is a modular pump, or is a polynary pump.
8. a kind of multidimensional liquid chromatographic separation system according to claim 4, which is characterized in that the high-efficient liquid phase color
Spectrum gradient pump A, high performance liquid chromatography gradient pump B are made of two modular pumps, or are made of a polynary gradient pump；It is described dilute
Releasing liquid pump is a modular pump, or is a polynary pump.
9. a kind of multidimensional liquid chromatographic separation system described according to claim 1 or 2 or 5 or 7 or 8, which is characterized in that described
Detector is various for detecting the device of chromatographic signal in separation process, includes but are not limited to UV detector, diode
Array detector, evaporative light scattering detector or mass detector can be one or more detector joints.
10. a kind of multidimensional liquid chromatographic separation system according to claim 6, which is characterized in that the detector is each
Plant the device for detecting chromatographic signal in separation process, include but are not limited to UV detector, diode array detector,
Evaporative light scattering detector or mass detector can be one or more detector joints.
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| PCT/CN2019/104868 WO2020052511A1 (en) | 2018-09-11 | 2019-09-09 | Multi-dimensional liquid chromatographic separation system |
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| CN109900840A (en) * | 2019-04-16 | 2019-06-18 | 李宜珊 | Multidimensional liquid chromatographic separation system based on double two position four-way valves |
| CN110025982A (en) * | 2019-04-22 | 2019-07-19 | 李宜珊 | Multidimensional liquid chromatographic separation system based on two ten-way valves |
| CN110672752A (en) * | 2019-10-21 | 2020-01-10 | 李宜珊 | Multidimensional liquid chromatography separation device |
| WO2020052511A1 (en) * | 2018-09-11 | 2020-03-19 | 李宜珊 | Multi-dimensional liquid chromatographic separation system |
| CN113495058A (en) * | 2021-07-31 | 2021-10-12 | 西安永瑞自动化有限公司 | Rare earth extraction online analysis system and analysis method thereof |
| CN114705776A (en) * | 2022-03-31 | 2022-07-05 | 苏州汇通色谱分离纯化有限公司 | Multidimensional liquid chromatography device and method for purifying ginkgetin |
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| CN208902668U (en) * | 2018-09-11 | 2019-05-24 | 李宜珊 | A kind of multidimensional liquid chromatographic separation system |
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| CN108037233A (en) * | 2017-12-28 | 2018-05-15 | 大连博迈科技发展有限公司 | The multidimensional liquid chromatographic separation system of full on-line checking based on same detector |
| CN208902668U (en) * | 2018-09-11 | 2019-05-24 | 李宜珊 | A kind of multidimensional liquid chromatographic separation system |
Cited By (8)
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| CN109900840A (en) * | 2019-04-16 | 2019-06-18 | 李宜珊 | Multidimensional liquid chromatographic separation system based on double two position four-way valves |
| CN110025982A (en) * | 2019-04-22 | 2019-07-19 | 李宜珊 | Multidimensional liquid chromatographic separation system based on two ten-way valves |
| CN110672752A (en) * | 2019-10-21 | 2020-01-10 | 李宜珊 | Multidimensional liquid chromatography separation device |
| CN113495058A (en) * | 2021-07-31 | 2021-10-12 | 西安永瑞自动化有限公司 | Rare earth extraction online analysis system and analysis method thereof |
| CN113495058B (en) * | 2021-07-31 | 2023-09-22 | 西安永瑞自动化有限公司 | Rare earth extraction online analysis system and analysis method thereof |
| CN114705776A (en) * | 2022-03-31 | 2022-07-05 | 苏州汇通色谱分离纯化有限公司 | Multidimensional liquid chromatography device and method for purifying ginkgetin |
| CN114705776B (en) * | 2022-03-31 | 2023-09-08 | 苏州汇通色谱分离纯化有限公司 | Method for purifying ginkgo flavone |
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