CN209148609U - A kind of three-dimensional liquid chromatographic separation system - Google Patents
A kind of three-dimensional liquid chromatographic separation system Download PDFInfo
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- CN209148609U CN209148609U CN201821563673.8U CN201821563673U CN209148609U CN 209148609 U CN209148609 U CN 209148609U CN 201821563673 U CN201821563673 U CN 201821563673U CN 209148609 U CN209148609 U CN 209148609U
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Abstract
The utility model relates to a kind of three-dimensional liquid chromatographic separation systems, including efficient liquid-phase chromatographic pump A, efficient liquid-phase chromatographic pump B, gradient mixer A, gradient mixer B, sampling valve, two ten-way valves, two six-way valves, enriching column array A, enriching column array B, liquid chromatography separation column array, detector, diluting pump, fraction collector and connecting line.The utility model carries out the switching of multidimensional discrete state by two ten-way valves and two six-way valves, realizes one-dimensional, two-dimentional or three-dimensional chromatogram separating capacity.This kind three-dimensional liquid chromatographic separation system scalability is strong, under the premise of not increasing system cost, it is only necessary to system pipeline reconnect can be upgraded to multidimensional liquid chromatographic separation system, system is made to have the more high-dimensional separating capacity such as four-dimensional chromatographic isolation；Common complete three-dimensional liquid chromatographic separation system can be become by reconnecting pipeline when needed again.There is boundless application prospect in the very high complex system sample separation analysis of separating difficulty.
Description
Technical field
The utility model belongs to high performance liquid chromatography separation technical field, is related to a kind of three dimension high efficiency liquid chromatogram segregative line
System.
Background technique
The limited resolution ratio and peak capacity that common one-dimensional chromatographic fractionation system can be provided are difficult to meet to extremely complicated
System sample carries out the requirement that full constituent separates, analyzes.Multi-dimensional chromatograph technology can greatly improve whole system peak capacity and
Separation selectivity can not replace in terms of solving complicated component, content unevenness, serious interference, component unknown sample with unique
The effect in generation has rapidly become one of the hot spot of chromatographic science research field.
The most common multidimensional liquid chromatogram interfacing has 3 kinds: the interfacing based on sample loop；Based on enriching column (
Claim trapping column) interfacing；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 respectively ties up chromatographic isolation independence, does not interfere with each other, using model
It encloses extensively.The quantity of enriching column is a key index of the system separating capacity in serial mode multidimensional liquid chromatographic system.
Serial mode multidimensional liquid chromatographic system matches the full-automatic high pass of spectrum Tyke (Sepiatec GmbH) company with Germany
Amount preparative separation system sepbox series of products are representative, but the product can only carry out Two way chromatograms separation, and separating capacity has
Limit.
Chinese patent application CN108037233A discloses a kind of multidimensional liquid of full on-line checking based on same detector
Phase chromatographic fractionation system.The system belongs to serial mode multidimensional liquid chromatographic system, and it is measurable and controllable to realize separation process whole process,
Enriching column and splitter clean-up performance can detecte, and the automation suitable for the very high complex sample system of separating difficulty repeats to divide
Analysis, separation and preparation, are easy to implement the efficient preparation of monomeric compound.But this kind of system is in Two way chromatograms clastotype
Whole enriching columns can not be used for the enrichment of component, do not play the efficiency of whole enriching columns.
Utility model content
The purpose of this utility model is being retained for some problems present in existing multidimensional liquid chromatogram isolation technics
On the basis of existing multidimensional liquid chromatogram isolation technics advantage, whole enriching columns can be played in two dimensional separation mode by providing one kind
Efficiency, and there is the Split liquid chromatographic apparatus of three-dimensional chromatographic isolation mode.
In order to achieve the above object, the technical solution of the utility model are as follows:
A kind of three-dimensional liquid chromatographic separation system, including efficient liquid-phase chromatographic pump A, efficient liquid-phase chromatographic pump B, gradient mixing
Device A, gradient mixer B, sampling valve, two ten-way valves, two six-way valves, enriching column array A, enriching column array B, liquid phase color
Compose splitter array, detector, efficient liquid phase diluting pump, collector 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 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 1. position of two six-way valves, 2. position, 3. position,
4. position, 5. position, 6. position only indicates syntople, it is not necessary to, number position name and sequence corresponding with the physical markings of two six-way valves
For since any interface of two ten-way valves according to it is counterclockwise or clockwise since 1. sort name；The detector is used for
Detect the chromatographic signal in separation process；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 same a period of time
There can only be a chromatography column conducting quarter；To being externally provided with a fixed entrance and a fixed outlet, and at least one
A straight-through bypass, the bypass and splitter are in parallel by multidigit selector valve；When by-path turn-on, other chromatography columns cannot
Conducting, when the conducting of other chromatography columns, bypass cannot be connected；The quantity of chromatography column determines as needed.
Enriching column array A, the enriching column array B is in parallel by multidigit selector valve by multiple chromatograph enrichment columns
At can only have the conducting of enriching column in synchronization；At least one straight-through bypass, the bypass and enriching column are selected by multidigit
Select valve parallel connection；When by-path turn-on, other enriching columns cannot be connected, and when the conducting of other enriching columns, bypass cannot be connected；It is right
Outer there are two interfaces, are respectively defined as interface X and interface Y；The quantity of enriching column determines as needed；The multiple enriching column battle array
Column can be with one in series multistage enriching column array, 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.
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 and the entrance of sampling valve connect, and the outlet of sampling valve is connect with the 1. position of two ten-way valves, and two ten
The 10. position of port valve is connect with the 7. position of two ten-way valves, and the 6. position of two ten-way valves and the entrance of liquid chromatography separation column array connect
It connecing, the outlet of liquid chromatography separation column array is connect with detector, and the outlet of detector is connect with the entrance of gradient mixer B,
Diluting pump is connect with the entrance of gradient mixer B, and the outlet of gradient mixer B is connect with the 8. position of two ten-way valves；Two
The 9. position of ten-way valve is connect with 4. position；The 5. position of two ten-way valves is connect with the 1. position of two six-way valves；Two six-way valves are 6.
Position is connect with the Y interface of enriching column array B, and the interface X of enriching column array B is connect with the 3. position of two six-way valves；Two six logical
The 2. position of valve is connect with the interface Y of enriching column array A, and the interface X of enriching column array A is connect with the 2. position of two ten-way valves；Two
The 3. position of position ten-way valve is connect with the 4. position of two six-way valves, the 5. position of two six-way valves and the entrance connection of fraction collector.
Based on the pipeline connecting mode of above-mentioned three-dimensional liquid chromatographic separation system, pass through two ten-way valves of control and two six
The state of port valve, realization system are converted to down one-dimensional discrete state from upper one-dimensional discrete state, it is achievable it is most it is three-dimensional it is complete
The chromatographic isolation function of line detection.
The sampling valve is a sampling device, can be two six logical switch sampling valves or sample injector；It can be
Other multidigits for realizing liquid or solid-state loading switch 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.
Compared with existing multi-dimensional chromatograph isolation technics, the utility model has the following beneficial effects:
(1) three-dimensional liquid chromatographic separation system constructed by the utility model is retaining existing multi-dimensional chromatograph isolation technics
On the basis of advantage, the efficiency of all enriching columns can be played in two-dimentional full constituent clastotype and focus objects are provided
The three-dimensional chromatogram separating capacity of component.Different chromatography column combinations is selected according to the difference of analyzed sample or fraction, system makes
It is flexible and convenient with control, it can be run under various modes, for example, one-dimensional clastotype, two dimensional separation mode, three-dimensional splitting die
Formula etc.；
(2) three-dimensional liquid chromatographic separation system scalability constructed by the utility model is strong, is not increasing system cost
Under the premise of, multidimensional liquid chromatographic separation system can be upgraded to by only needing to reconnect system pipeline at the scene, have system
The more high-dimensional separating capacities such as standby four-dimension chromatographic isolation mode；Pipeline can be reconnected again when needed becomes common complete
Three-dimensional liquid chromatographic separation system.Before having boundless application in the very high complex system sample separation analysis of separating difficulty
Scape.
(3) three-dimensional liquid chromatographic separation system constructed by the utility model, the entrance and exit of enriching column array are not
Fixed, in the second dimension chromatographic separation process, when enriching column is as loading column, the flow direction of eluent and richness originally
Collect sample when mobile phase flow direction on the contrary, and sample is generally enriched in the entrance of enriching column, it is therefore desirable to less stream
It is dynamic mutually and less time complete the elution and loading of sample in enriching column and then to reduce total disengaging time, it improves point
From efficiency.
Detailed description of the invention
Fig. 1 a, Fig. 1 b is that the pipeline that three-dimensional liquid chromatographic separation system first provided by the utility model ties up discrete state connects
Binding composition, two ten-way valves are A condition in Fig. 1 a and Fig. 1 b, and two six-way valves are A condition in Fig. 1 a, two six in Fig. 1 b
Port valve is B state.
Fig. 2 is the pipe of the three-dimensional dimension of liquid chromatographic separation system first or the second dimension discrete state provided by the utility model
Road connection structure diagram.Wherein, two ten-way valves are B state, and two six-way valves are B state.
Fig. 3 is the first dimension, the pipeline connecting figure of the second dimension or third dimension chromatographic isolation state, wherein two ten-way valves are
B state, two six-way valves are A condition.
Fig. 4 is the pipeline jointing construction figure of liquid chromatography separation column array.
Fig. 5 is the pipeline jointing construction figure of enriching column array A, enriching column array B.
Fig. 6 a is two six-way injection valve sample loading condition (LOAD state, A condition) pipeline jointing construction figures, the state
Lower that sample is loaded into quantitative loop, wherein 4. position is defined as the entrance of sampling valve, 5. position is defined as the outlet of sampling valve；
Fig. 6 b is two six-way injection valve sample loading condition (INJECT state, B state) pipeline jointing construction figures, the shape
Sample will be separated from being injected into separation system flow path in quantitative loop under state, wherein 4. position is defined as the entrance of sampling valve,
5. position is defined as the outlet of sampling valve.
Fig. 7 is the three dimension high efficiency liquid chromatographic separation system structure chart of the utility model embodiment.
Specific embodiment
Embodiments discussed below is only a kind of description applied to the utility model patent, not to the utility model
Range be defined, under the premise of not departing from the spirit of the design of the utility model, those of ordinary skill in the art are to this is practical
The various changes and improvements that New Scheme is made should all fall into the protection scope that the utility model claims book determines.
It is a kind of three-dimensional 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, two six-way valves and connecting line.Wherein, diluting pump is efficient
Liquid phase diluting 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 and the entrance of sampling valve connect, and the outlet of sampling valve is connect with the 1. position of two ten-way valves, and two ten
The 10. position of port valve is connect with the 7. position of two ten-way valves, and the 6. position of two ten-way valves and the entrance of liquid chromatography separation column array connect
It connecing, the outlet of liquid chromatography separation column array is connect with detector, and the outlet of detector is connect with the entrance of gradient mixer B,
Diluting pump is connect with the entrance of gradient mixer B, and the outlet of gradient mixer B is connect with the 8. position of two ten-way valves；Two
The 9. position of ten-way valve is connect with 4. position；The 5. position of two ten-way valves is connect with the 1. position of two six-way valves；Two six-way valves are 6.
Position is connect with the Y interface of enriching column array B, and the interface X of enriching column array B is connect with the 3. position of two six-way valves；Two six logical
The 2. position of valve is connect with the interface Y of enriching column array A, and the interface X of enriching column array A is connect with the 2. position of two ten-way valves；Two
The 3. position of position ten-way valve is connect with the 4. position of two six-way valves, the 5. position of two six-way valves and the entrance connection of fraction collector.
It further illustrates with reference to the accompanying drawing.
Two ten-way valves are A condition in Fig. 1 a, and two six-way valves are A condition.At this point, high performance liquid chromatography gradient pump A and
High performance liquid chromatography gradient pump B and gradient mixer A forms chromatographic isolation gradient elution mobile phase feed system, gradient mixer
The outlet of A is connect with sampling valve, and the outlet of sampling valve is connect with the 1. position of two ten-way valves；The 1. position of two ten-way valves and 10. position
Conducting, the 10. position of two ten-way valves is connect with 7. position；The 7. position of two ten-way valves is connected with 6. position, the 6. position of two ten-way valves with
The entrance of splitter array connects, and the outlet of splitter array and the entrance of detector connect, and detector detects chromatographic signal, inspection
The outlet for surveying device is connect with the entrance of gradient mixer B, and diluting pump is connect with the entrance of gradient mixer B, is mixed through gradient
Sample is flowed out after device B dilution column, outlet is connect with the 8. position of two ten-way valves；The 8. position of two ten-way valves is connected with 9. position,
The 9. position of two ten-way valves is connect with 4. position；The 4. position of two ten-way valves is connected with 5. position, the 5. position of two ten-way valves with two
The 1. position of six-way valve connects, and the 1. position of two six-way valves is connected with the 6. position of two six-way valves；The 6. position of two six-way valves and richness
Interface Y (entrance that interface Y is enriching column array B at this time) connection of clustered column array B, the interface X of enriching column array B (connect at this time
The outlet that mouth X is enriching column array B) it is connect with the 3. position of two six-way valves；The 3. position of two six-way valves and two six-way valves
2. position is connected；The 2. position of two six-way valves and the interface Y (entrance that interface Y is enriching column array A at this time) of enriching column array A
The interface X (outlet that interface X is enriching column array A at this time) of connection, enriching column array A is connect with the 2. position of two ten-way valves,
Realize the enrichment of sample；The 2. position of two ten-way valves is connected with 3. position, the 4. position of the 3. position of two ten-way valves and two six-way valves
Connection；The 4. position of two six-way valves is connected with the 5. position of two six-way valves, two 5. positions of six-way valve and entering for fraction collector
Mouth connection, realizes sample collection.
Two ten-way valves are A condition in Fig. 1 b, and two six-way valves are B state.At this point, high performance liquid chromatography gradient pump A and
High performance liquid chromatography gradient pump B and gradient mixer A forms chromatographic isolation gradient elution mobile phase feed system, gradient mixer
The outlet of A is connect with sampling valve, and the outlet of sampling valve is connect with the 1. position of two ten-way valves；The 1. position of two ten-way valves and 10. position
Conducting, the 10. position of two ten-way valves is connect with 7. position；The 7. position of two ten-way valves is connected with 6. position；The 6. position of two ten-way valves with
The entrance of splitter array connects, and the outlet of splitter array and the entrance of detector connect, and detector detects chromatographic signal, inspection
The outlet for surveying device is connect with the entrance of gradient mixer B, and diluting pump is connect with the entrance of gradient mixer B, is mixed through gradient
Sample is flowed out after device B dilution column, outlet is connect with the 8. position of two ten-way valves；The 8. position of two ten-way valves is connected with 9. position,
The 9. position of two ten-way valves is connect with 4. position；The 4. position of two ten-way valves is connected with 5. position, the 5. position of two ten-way valves with two
The 1. position of six-way valve connects；The 1. position of two six-way valves is connected with the 2. position of two six-way valves；The 2. position of two six-way valves and richness
Interface Y (entrance that interface Y is enriching column array A at this time) connection of clustered column array A, the interface X of enriching column array A (connect at this time
The outlet that mouth X is enriching column array A) it is connect with the 2. position of two ten-way valves；The 2. position of two ten-way valves is connected with 3. position, and two
The 3. position of position ten-way valve is connect with the 4. position of two six-way valves；The 4. position of two six-way valves is connected with the 3. position of two six-way valves,
The 3. position of two six-way valves is connect with the interface X (entrance that interface X is enriching column array B at this time) of enriching column array B, is enriched with
The interface Y (outlet that interface Y is enriching column array B at this time) of column array B is connect with the 6. position of two six-way valves；Two six logical
The 6. position of valve is connected with 5. position, and the 5. position of two six-way valves and the entrance of fraction collector connect, and realizes sample collection.
Two ten-way valves are B state in Fig. 2, and two six-way valves are B state.At this point, high performance liquid chromatography gradient pump A and height
Effect liquid phase chromatogram gradient pump B and gradient mixer A forms chromatographic isolation gradient elution mobile phase feed system, gradient mixer A
Outlet connect with sampling valve, the outlet of sampling valve is connect with the 1. position of two ten-way valves；The 1. position of two ten-way valves and 2. position
It is connected and is connect with the interface X of enriching column array A (entrance that interface X is enriching column array A at this time), enriching column array A's connects
Mouth Y (outlet that interface Y is enriching column array A at this time) is connect with the 2. position of two six-way valves；The 2. position of two six-way valves with 1.
Position conducting, the 1. position of two six-way valves is connect with the 5. position of two ten-way valves；The 5. position of two ten-way valve A is connected with 6. position；Two
The 6. position of position ten-way valve is connect with the entrance of splitter array, and the outlet of splitter array and the entrance of detector connect, detection
Device detects chromatographic signal, and the outlet of detector is connect with the entrance of gradient mixer B, and diluting pump enters with gradient mixer B's
Mouth connection, flows out sample after gradient mixer B dilutes column, and outlet is connect with the 8. position of two ten-way valves；Two ten-way valves
8. position be connected with 7. position, the 7. position of two ten-way valves is connect with 10. position；The 10. position of two ten-way valves is connected with 9. position, and two ten
The 9. position of port valve is connect with 4. position；The 4. position of two ten-way valves is connected with 3. position；The 3. position of two ten-way valves and two six-way valves
4. position connection；The 4. position of two six-way valves is connected with 3. position, the 3. position of two six-way valves and interface X (this of enriching column array B
When interface X be enriching column array B entrance) connection, (interface X is enriching column array B to the interface Y of enriching column array B at this time
Outlet) it is connect with the 6. position of two six-way valves；The 6. position of two six-way valves is connected with 5. position, the 5. position of two six-way valves and fraction
The entrance of collector connects, and realizes sample collection.
Two ten-way valves are B state in Fig. 3, and two six-way valves are A condition.At this point, high performance liquid chromatography gradient pump A and height
Effect liquid phase chromatogram gradient pump B and gradient mixer A forms chromatographic isolation gradient elution mobile phase feed system, gradient mixer A
Outlet connect with sampling valve, the outlet of sampling valve is connect with the 1. position of two ten-way valves；The 1. position of two ten-way valves and 2. position
It is connected and is connect with the interface X of enriching column array A (entrance that interface X is enriching column array A at this time), enriching column array A's connects
Mouth Y (outlet that interface X is enriching column array A at this time) is connect with the 2. position of two six-way valves；The 2. position of two six-way valves with 3.
Position conducting, the 3. position of two six-way valves and the interface X (entrance that interface X is enriching column array B at this time) of enriching column array B connect
It connects, the interface Y (entrance that interface Y is enriching column array B at this time) of enriching column array B is connect with the 6. position of two six-way valves；Two
The 6. position of position six-way valve is connected with 1. position, and the 1. position of two six-way valves is connect with the 5. position of two ten-way valves；Two ten-way valves
5. position is connected with 6. position, the 6. position of two ten-way valves is connect with the entrance of splitter array, the outlet and detection of splitter array
The entrance of device connects, and detector detects chromatographic signal, and the outlet of detector is connect with the entrance of gradient mixer B, diluting pump
It is connect with the entrance of gradient mixer B, sample is flowed out after gradient mixer B dilutes column, outlet and two ten-way valves are 8.
Position connection；The 8. position of two ten-way valves is connected with 7. position, and the 7. position of two ten-way valves is connect with 10. position；The 10. position of two ten-way valves
It is connected with 9. position, the 9. position of two ten-way valves is connect with 4. position；The 4. position of two ten-way valves is connected with 3. position, two ten-way valves
3. position is connect with the 4. position of two six-way valves；The 4. position of two six-way valves is connected with 5. position, the 5. position of two six-way valves and fraction
The entrance of collector connects, and realizes sample collection.
A kind of three dimension high efficiency liquid chromatographic separation system structure of embodiment
Enriching column array A is two-stage enriching column array in the embodiment, and every grade of enriching column array has 9 enriching columns, i.e., rich
Clustered column array A be 18 enriching columns, number consecutively be enriching column array A the 1st enriching column, the 2nd enriching column, etc., last
The 18th enriching column that a number is enriching column array A；Enriching column array B has 9 enriching columns, and number consecutively is enriching column array B
The 1st enriching column, the 2nd enriching column, etc., the 9th enriching column that the last one number is enriching column array B；Liquid chromatogram separation
Column array has 5 splitters, and number consecutively is the 1st splitter, and the 2nd splitter, etc., last root is the 5th splitter；Referring to
Fig. 7.
The following are the operation of above-mentioned three dimension high efficiency liquid chromatographic separation system structure explanations:
The three dimension high efficiency liquid chromatographic system primary operating mode is Enrichment Mode and clastotype and these modes
Combination.In practical applications, it selects as required.It is briefly described as follows.
1. Enrichment Mode
Selective absorption and gradient elution, Enrichment Mode based on enrichment column packing can both retain main component, remove
Impurity composition, be mainly used for target components divides the analysis of variance；Can also retain trace, remove main component, reduce trace at
The detection limit divided, improves the detection level of trace constituent, is mainly used for target impurity identification and analysis and unknown impuritie discovery.
Enrichment Mode includes single Enrichment Mode and double Enrichment Modes.Single Enrichment Mode be repeated several times by sampling valve into
Sample realizes the enrichment of a kind of target components using the selective absorption of enriching column array A or enriching column array B, referring to fig. 2 and
Fig. 3.Double Enrichment Modes are that sample introduction is repeated several times by sampling valve, are utilized respectively the selection of enriching column array A and enriching column array B
Property absorption, realize two class target components enrichment, referring to figs. 2 and 3.
2. one-dimensional separation system operational mode
One-dimensional separation system operational mode includes clastotype, Rich Internet Applications mode, Rich Internet Applications-Enrichment Mode and divides
From-Enrichment Mode etc..
Clastotype is to carry out chromatography point using a splitter in chromatography column array by sample introduction valve injection
From using the collection of collector progress target components, referring to Fig. 1 a and Fig. 1 b.Wherein, enriching column array A and enriching column array B
It is in by-path turn-on state.
Rich Internet Applications mode is that the enrichment of target components is carried out first with enriching column array A, recycles chromatography column battle array
A splitter in column carries out chromatographic isolation, is collected using the cutting that collector carries out target components, at this point, enriching column array
B is in by-path turn-on state.Referring to fig. 2.
Rich Internet Applications-Enrichment Mode is the enrichment that target components are carried out first with enriching column array A, recycles chromatography point
Chromatographic isolation is carried out from a splitter in column array, the enrichment of target components is finally carried out using enriching column array B.Referring to
Fig. 2.
Separation-Enrichment Mode is that sample introduction is repeated several times using sampling valve, utilizes a separation in chromatography column array
Column carries out chromatographic isolation, and enriching column array A or enriching column array B is recycled to carry out the enrichment of target components.Referring to Fig. 1 a and figure
1b.The mode most multipotency is enriched with 27 components.
3. two dimensional separation system running pattern
Two dimensional separation system running pattern tool includes separation-Rich Internet Applications mode and Rich Internet Applications-Rich Internet Applications mould
Formula.
Separation-Rich Internet Applications mode is that sample introduction is repeated several times first with sampling valve, using in chromatography column array
One splitter carries out chromatographic isolation, and enriching column array A and enriching column array B is recycled successively to carry out the enrichment of target components,
Most multipotency is enriched with 27 components, referring to Fig. 1 a；Then, 1 enriching column in enriching column array A or enriching column array B is selected to make
For sample column, the second dimension chromatographic isolation is carried out using another splitter in splitter array when sample column conducting,
The component needed is collected using collector, referring to Fig. 3.Separation-Rich Internet Applications mode can also develop as separation-enrichment-point
From-Enrichment Mode, in such cases, 18 components are enriched with using enriching column array A most multipotency when first time separation and concentration, second
Enriching column array B most multipotency is enriched with 9 components when secondary separation and concentration.
Rich Internet Applications-Rich Internet Applications mode is that sample introduction is repeated several times first with sampling valve, and target components are utilized richness
Clustered column array A is enriched with, at this point, chromatography column array and enriching column array B are in bypass condition, referring to fig. 2；Then
Select 1 enriching column in enriching column array A as sample column, when sample column conducting using in chromatography column array
One splitter carries out the first dimension chromatographic isolation, is successively enriched with the component of needs using enriching column array B, altogether can be rich
Collect 9 components, referring to fig. 2；Finally, selecting 1 enriching column in enriching column array B as sample column, when the sample column is connected
Another splitter in Shi Liyong splitter array carries out the second dimension chromatographic isolation, and the component of needs is received using collector
Collection, enriching column array A is in by-path turn-on state at this time, referring to Fig. 3.
4. three-dimensional clastotype
Three-dimensional clastotype refers to separation-Rich Internet Applications-Rich Internet Applications mode.Firstly, being repeated several times by sampling valve
Sample introduction carries out the first dimension chromatographic isolation, fraction is pressed using a splitter in chromatography column array, such as the 1st splitter
According in 18 enriching columns for needing successively to be enriched to enriching column array A, enriching column array B is in by-path turn-on state at this time, ginseng
See Fig. 1 a and Fig. 1 b；Then, two ten-way valves go to B state, select 1 enriching column in enriching column array A as sample
Column starts the second dimension chromatographic isolation when sample column conducting, fraction is successively enriched to the 9 of enriching column array B as required
In a enriching column, referring to fig. 2；Finally, two six-way valves are gone to A condition, by-path turn-on is in referring to Fig. 3, enriching column array A
State selects 1 enriching column in enriching column array B as sample column, starts third dimension color when sample column conducting
Spectrum separation successively collects fraction using collector as required.
Claims (3)
1. a kind of three-dimensional liquid chromatographic separation system, it is characterised in that: by efficient liquid-phase chromatographic pump A, efficient liquid-phase chromatographic pump B,
Gradient mixer A, gradient mixer B, sampling valve, two ten-way valves, two six-way valves, enriching column array A, enriching column array B,
Liquid chromatography separation column array, detector, efficient liquid phase diluting pump, fraction collector and connecting line are constituted；
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 indicate adjacent
Connect relationship, it is not necessary to which corresponding with the physical markings of two ten-way valves, number position is named and be ordered as to connect from two any of ten-way valve
Mouth starts according to the counterclockwise or sequence name since 1. clockwise；The 1. position of two six-way valves, 2. position, 3. position, 4. position,
5. position, 6. position only indicates syntople, it is not necessary to which corresponding with the physical markings of two six-way valves, number position is named and is ordered as from two
Any interface of position six-way valve starts according to the counterclockwise or sequence name since 1. clockwise；The detector divides for detecting
From chromatographic signal in the process；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 at least one is straight
Logical 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；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 straight-through bypass, the bypass and enriching column pass through multidigit selector valve
It is in parallel；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 interfaces, are respectively defined as interface X and interface Y；The quantity of enriching column determines as needed；
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 the 1. position of two ten-way valves, two ten-way valves
10. position connect with the 7. position of two ten-way valves, the 6. 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 is connect with detector, and the outlet of detector is connect with the entrance of gradient mixer B, dilution
Liquid pump is connect with the entrance of gradient mixer B, and the outlet of gradient mixer B is connect with the 8. position of two ten-way valves；Two ten logical
The 9. position of valve is connect with 4. position；The 5. position of two ten-way valves is connect with the 1. position of two six-way valves；The 6. position of two six-way valves with
The Y interface of enriching column array B connects, and the interface X of enriching column array B is connect with the 3. position of two six-way valves；Two six-way valves
2. position is connect with the interface Y of enriching column array A, the interface X of enriching column array A is connect with the 2. position of two ten-way valves；Two ten
The 3. position of port valve is connect with the 4. position of two six-way valves, and the 5. position of two six-way valves and the entrance of fraction collector connect；
By controlling the state of two ten-way valves and two six-way valves, realization system is converted to down one-dimensional from upper one-dimensional discrete state
Discrete state, it can be achieved that at most three-dimensional full on-line checking chromatographic isolation function.
2. a kind of three-dimensional liquid chromatographic separation system according to claim 1, which is characterized in that the multiple enriching column battle array
Column 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 is led all in bypass
It is logical.
3. a kind of three-dimensional liquid chromatographic separation system according to claim 1, which is characterized in that the detector is various
For detecting the device of chromatographic signal in separation process, UV detector is included but are not limited to, diode array detector is steamed
Light Scattering Detector or mass detector, the combined detection system including multiple detectors composition.
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