CN110133162A - Multidimensional liquid chromatographic separation system based on two multiple-way valves - Google Patents
Multidimensional liquid chromatographic separation system based on two multiple-way valves Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 42
- 238000013375 chromatographic separation Methods 0.000 title claims abstract description 23
- 238000000926 separation method Methods 0.000 claims abstract description 66
- 238000005070 sampling Methods 0.000 claims abstract description 32
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 26
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 20
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 20
- 238000007865 diluting Methods 0.000 claims abstract description 17
- 238000007445 Chromatographic isolation Methods 0.000 claims abstract description 7
- 239000007791 liquid phase Substances 0.000 abstract description 6
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000010828 elution Methods 0.000 abstract description 4
- 230000005526 G1 to G0 transition Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 238000012544 monitoring process Methods 0.000 abstract 1
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000010276 construction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000003480 eluent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000004012 multidimensional HPLC Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 239000004615 ingredient Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- -1 eluant Substances 0.000 description 1
- 238000000105 evaporative light scattering detection Methods 0.000 description 1
- 238000003818 flash chromatography Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
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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
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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 multiple-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 multi-pass Vavle 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, common multidimensional liquid chromatographic separation system mainly includes two kinds, the first is continuous loop switch type two dimension
Liquid chromatographic system belongs to analytic type multidimensional liquid chromatographic system；Second is serial mode multidimensional liquid chromatographic system, is belonged to
Preparative multidimensional liquid chromatographic system.
The full-automatic high-throughput preparation of United States Patent (USP) US6080318A and match spectrum Tyke (Sepiatec GmbH) company, Germany
Type separation system sepbox series of products are serial mode multidimensional liquid chromatographic system, can be carried out two-dimensional HPLC separation.
Chinese patent application CN105999765A discloses a kind of two-dimensional HPLC separation system.Chinese patent application
CN105938130A discloses a kind of two-dimensional HPLC separation system based on two eight ways valves.
Currently, serial mode multidimensional liquid chromatographic system has evolved into the serial multidimensional liquid chromatographic separation system of circulation,
The three-dimensional or three-dimensional above liquid chromatogram separating capacity can be provided, the efficient preparation of monomeric compound is easy to implement.Chinese patent Shen
Please CN108037233A disclose a kind of multidimensional liquid chromatographic separation system based on two ten-way valves；Chinese patent application
CN109557219A and CN109655561A individually discloses one kind based on two ten-way valves and there is enriching column reversely to elute function
Can multidimensional liquid chromatographic separation system, these systems while the three-dimensional or three-dimensional above liquid chromatogram separating capacity is provided,
Disengaging time and mobile phase can be saved to a certain extent.It is based in addition, Chinese patent application CN109557221A discloses one kind
The multidimensional liquid chromatographic separation system of two eight ways valves, Chinese patent application CN109541090A disclose a kind of based on two double
The multidimensional liquid chromatographic separation system of four-way valve.CN108037233A, CN109557219A, CN109655561A,
CN109557221A, CN109541090A, the sampling valve in above-mentioned patent is all connected to before enriching column array or enriching column battle array
In the bypass of column.
Summary of the invention
The object of the present invention is to provide a kind of sampling valve be connected to after enriching column array liquid chromatography separation column array it
Preceding multidimensional liquid chromatographic separation system meets the three-dimensional or three-dimensional above chromatographic isolation needs.
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, which is characterized in that the multidimensional liquid chromatographic separation system includes height
Effect liquid phase chromatogram gradient pump A, high performance liquid chromatography gradient pump B, diluting pump, gradient mixer A, gradient mixer B, sample introduction
Valve, enriching column array A, enriching column array B, fraction collector, liquid chromatography separation column array, detector, two multiple-way valves with
And connecting line；The detector is used to 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, can only have a color in synchronization
Compose splitter conducting；To being externally provided with a fixed entrance and a fixed outlet, and at least one is bypassed, the bypass and
Splitter is in parallel；When by-path turn-on, other chromatography columns cannot be connected, and when the conducting of other chromatography columns, bypass will
It 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, in synchronization
There can be an enriching column conducting；At least one bypass, the bypass and enriching column are in parallel；When by-path turn-on, other enriching columns will
It cannot be connected, when the conducting of other enriching columns, bypass cannot be connected；The quantity of enriching column determines as needed；There are two externally
Interface is respectively defined as interface X and interface Y.
The entrance of the sampling valve is connect with a port of two multiple-way valves, and the outlet of sampling valve is separated with liquid chromatogram
The entrance of column array connects, and the outlet of liquid chromatography separation column array is connect with detector.
By the state switching of two multiple-way valves of control, realization system is converted to down one-dimensional separation from upper one-dimensional discrete state
State completes cyclical chromatography function, realizes the chromatographic isolation function of the full on-line checking of multidimensional.
Two multiple-way valves described in above-mentioned multidimensional liquid chromatographic separation system include two ten-way valves, two eight ways valves and double
Two position four-way valves, including by multiple valve groups at and according to two ten-way valves or two eight ways valves or double two position four-way valves principles
The valve group of operation is closed.
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
Survey device, diode array detector, evaporative light scattering detector or mass detector, including multiple detector combined measurements system
System.
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.
Innovative point and beneficial effect of the invention is:
The entrance of sampling valve is connect with a port of two multiple-way valves, the outlet and liquid chromatography separation column battle array of sampling valve
The entrance of column connects, and the outlet of liquid chromatography separation column array is connect with detector.It, can low cost building energy based on above-mentioned connection
Meet the serial multidimensional liquid chromatographic separation system of circulation of chromatographic isolation needs.
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 position four-way valve A and two position four-way valve B 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 position four-way valve A and two position four-way valve B are B state；
Fig. 3 is the structure chart of liquid chromatography separation column array；
Fig. 4 is the structure chart of enriching column array A, enriching column array B；
Fig. 5 is column array element operating structure figure made of chromatography column or enriching column and two position four-way valve piping connections；
Fig. 5 (a) is column array element structure chart made of chromatography column or enriching column and two position four-way valve piping connections,
Wherein chromatography column or enriching column are on state, 1. port and 4. port definition is column array element external interface；
Fig. 5 (b) is column array element structure chart made of chromatography column or enriching column and two position four-way valve piping connections,
Wherein chromatography column or enriching column are nonconducting state, 1. port and 4. port definition is column array element external interface；
Fig. 6 is the piping connection and operating structure figure of two six-way injection valves；
Fig. 6 (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. port definition is the entrance of sampling valve, 5. port definition is going out for sampling valve
Mouthful；
Fig. 6 (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. port definition is entering for sampling valve
Mouthful, 5. port definition is the outlet of sampling valve；
Fig. 7 (a) is the Multidimensional HPLC separation system structure chart of the embodiment of the present invention, two position four-way valve A and two
Position four-way valve B is A condition, and the first splitter is on state, and the first enriching column in enriching column array A is on state；
In Fig. 7 (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 liang of position four-way valve A, 13 liang of position four-way valve B；
Fig. 7 (b) is the Multidimensional HPLC separation system structure chart of the embodiment of the present invention, two position four-way valve A and two
Position four-way valve B is B 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, double two position four-way valves and connecting line.Wherein, double two position four-way valves are skills of the present invention
Two multiple-way valves in art scheme are made of two position four-way valve A, two position four-way valve B and according to a double two position four-way valve principles
Operation；Enriching column array A, enriching column array B are the unit string being formed by connecting by two position four-way valves and an enriching column
Connect composition；Liquid chromatography separation column array is the unit concatenation group being formed by connecting by two position four-way valves and a splitter
At；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 is connect with the 1. port of two position four-way valve A, the 2. port of two position four-way valve A and enriching column array B
The connection of X interface, the Y interface of enriching column array B connect with the 2. port of two position four-way valve B, the 1. port of two position four-way valve B and
The entrance of sampling valve connects, and the outlet of sampling valve is connect with the entrance of liquid chromatography separation column array, liquid chromatography separation column battle array
The outlet of column is connect with detector, and the outlet of detector is connect with the entrance of gradient mixer B, diluting pump and gradient mixer
The entrance of B connects, and the outlet of gradient mixer B is connect with the 3. port of two position four-way valve B, the 4. port of two position four-way valve B and
The Y interface of enriching column array A connects, and the X interface of enriching column array A is connect with the 4. port of two position four-way valve A, two ten-way valves
3. port and fraction collector entrance connect.Two position four-way valve A and two position four-way valve B 1., 2., 3., 4. port only table
Show syntople, it is not necessary to it is corresponding with the physical markings of two position four-way valve A and two position four-way valve B, port name and be ordered as from
The arbitrary port of two position four-way valve A and two position four-way valve B start according to the counterclockwise or sequence name since 1. clockwise.
Two position four-way valve A and two position four-way valve B are A condition in Fig. 1, at this point, high performance liquid chromatography gradient pump A and efficiently
Liquid chromatogram gradient pump B and gradient mixer A forms chromatographic isolation gradient elution mobile phase feed system, gradient mixer A's
Outlet is connect with the 1. port of two position four-way valve A；The 1. port of two position four-way valve A be connected with 2. port and with enriching column array B
Interface X (at this time the interface X of enriching column array B be its entrance) connection；Interface Y (the enriching column battle array at this time of enriching column array B
The interface Y of column B exports for it) connect with the 2. port of two position four-way valve B, the 2. port of two position four-way valve B is connected with 1. port；Two
The 1. port of position four-way valve B and the entrance of sampling valve connect, and the outlet of sampling valve and the entrance of liquid chromatography separation column array connect
It connects；Any chromatographic column in selection splitter array is separated；The outlet of splitter array is connect with detector, detector inspection
The outlet of colour examining spectrum signal, detector is connect with the entrance of gradient mixer B, and the entrance of diluting pump and gradient mixer B connect
It connects, sample is flowed out after gradient mixer B dilutes column, the outlet gradient mixer B is connect with the 3. port of two position four-way valve B；Two
The 3. port of position four-way valve B is connected with 4. port；The 4. port of two position four-way valve B and the interface Y of enriching column array A are (rich at this time
The interface Y of clustered column array B is its entrance) connection, (the interface X of enriching column array A is it to the interface X of enriching column array A at this time
Outlet) it is connect with the 4. port of two position four-way valve A, realize the enrichment of separation sample；The 4. port of two position four-way valve A and 3. port
Conducting, the 3. port of two position four-way valve A and the entrance of fraction collector connect, and realize sample collection.
Two position four-way valve A and two position four-way valve B are B state in Fig. 2.At this point, high performance liquid chromatography gradient pump A and efficiently
Liquid chromatogram gradient pump B and gradient mixer A forms chromatographic isolation gradient elution mobile phase feed system, gradient mixer A's
Outlet is connect with the 1. port of two position four-way valve A, and the 1. port of two position four-way valve A is connected with 4. port；Two position four-way valve A's
4. port connect (the interface X of enriching column array A is its entrance at this time) with the interface X of enriching column array A；Enriching column array A's
Interface Y (the interface Y of enriching column array A exports at this time for it) is connect with the 4. port of two position four-way valve B；Two position four-way valve B's
4. port is connected with 1. port, the 1. port of two position four-way valve B and the entrance of sampling valve are connected, the outlet of sampling valve and liquid phase color
Compose the entrance connection of splitter array；Any chromatographic column in selection splitter array is separated；The outlet of splitter array
It is connect with detector, 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, gradient mixer B is exported and two four
The 3. port of port valve B connects；The 3. port of two position four-way valve B is connected with 2. port；The 2. port of two position four-way valve B and enriching column
The interface Y connection of array B (the interface Y of enriching column array B is its entrance at this time)；The interface X of enriching column array B is (rich at this time
The interface X of clustered column array B exports for it) it is connect with the 2. port of two position four-way valve A, realize the enrichment of separation sample；Two four
The 2. port of port valve A is connected with 3. port；The 3. port of two position four-way valve A and the entrance of fraction collector connect, and realize sample
It collects.
A kind of embodiment: multidimensional liquid chromatographic separation system structure
Enriching column array B has 9 enriching columns in the embodiment, the 1st enriching column that number consecutively is enriching column array B, the
2 enriching columns, etc., the 9th enriching column that the last one number is enriching column array B；Enriching column array A has 18 enriching columns, according to
The 1st enriching column that secondary number is enriching column array A, the 2nd enriching column, etc., the last one number is the 18th of enriching column array A
Enriching column；Liquid chromatography separation column array has 4 splitters, and number consecutively is the 1st splitter, the 2nd splitter, etc., finally
One is the 4th splitter；Four-way valve A and two position four-way valve B in Fig. 7 (a) are A condition, the four-way valve A in Fig. 7 (b) and
Two position four-way valve 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 position four-way valve A and two position four-way valve B are A condition, referring to Fig. 1；Enriching column
Array B 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 are connected manually；When sampling valve is switched to INJECT state, start the first dimension separation；It is diluting
Under liquid pump is assisted, according to properties of samples and detection signal successively by fraction using in the 1st to the 9th enriching column of enriching column array A
It is enriched with, use when the 10th to the 18th enriching column of enriching column array A gives over to third dimension separation；Repeatedly, until enrichment
There are enough compounds in the 1st to the 9th enriching column of column array A, is transferred to the second dimension separation process control；If be not required to
Two dimensional separation is wanted, then enriching column array A is constantly in bypass condition, and the receipts of multiple fractions are directly carried out using fraction collector
Collection.
Second dimension separation process control: after the first dimension separation process control, sampling valve should switch to LOAD shape
State, two position four-way valve A and two position four-way valve B switch to B state, referring to fig. 2；Selection the second dimension chromatography column, for example, the
2 splitters, the chromatography column are connected manually；An enriching column in the 1st to the 9th enriching column of enriching column array A is selected to make
For the sample column of two dimensional separation；When enriching column conducting, the second dimension separation process starts；Under diluting pump assistance, root
Successively fraction is switched to according to properties of samples and detection signal in the 1st to the 9th enriching column of enriching column array B and is enriched with；Such as
Fruit does not need third dimension separation, then can successively elute the 1st to the 9th enriching column of enriching column array B, straight using fraction collector
Tap into the collection of the multiple fractions of row；Repeatedly, two dimensional separation is completed；
Third dimension separation process control: after the second dimension separation process control, two position four-way valve A and two position four-way valve B
A condition is all switched to, referring to Fig. 1；Sampling valve keeps LOAD state；Third dimension chromatography column is selected, for example, the 3rd splitter,
The chromatography column is connected manually；Select an enriching column in the 1st to the 9th enriching column of enriching column array B as the third dimension
Isolated sample column；When enriching column conducting, third dimension separation process starts；If necessary to carry out fourth dimension separation, then exist
Under diluting pump is assisted, fraction is successively switched to the 10th to the 18th of enriching column array A the according to properties of samples and detection signal
It is enriched in enriching column, is 9 parts by faction cut；If you do not need to carry out fourth dimension separation, then it can be by enriching column array B's
1st to the 9th enriching column successively elutes separation, and the collection of multiple fractions is directly carried out using fraction collector；Repeatedly, it completes
Third dimension separation.
Fourth dimension separation process control: after third dimension separation process controls, two position four-way valve A and two position four-way valve B
B state is all switched to, referring to fig. 2；Sampling valve keeps LOAD state；Fourth dimension chromatography column is selected, for example, the 4th splitter,
The chromatography column is connected manually；Select an enriching column in the 10th to the 18th enriching column of enriching column array A as the 4th
Tie up isolated sample column；When enriching column conducting, fourth dimension separation process starts；Under gradient eluent effect, it can will make
Fourth dimension separation is carried out under the effect of the 4th splitter for the compound elution in the enriching column of sample column；Utilize Fraction collection
Device is collected multiple fractions；Repeatedly, fourth dimension separation is completed.
Claims (2)
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 multiple-way valves and company
Take over road；The detector is used to 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, can only have chromatography point in synchronization
It is connected from column；To being externally provided with a fixed entrance and a fixed outlet, and at least one is bypassed, the bypass and separation
Column is in parallel；When by-path turn-on, other chromatography columns cannot be connected, and when the conducting of other chromatography columns, bypass cannot
Conducting；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, can only be had in synchronization
One enriching column conducting；At least one bypass, the bypass and enriching column are in parallel；When by-path turn-on, other enriching columns cannot
Conducting, when the conducting of other enriching columns, bypass cannot be connected；The quantity of enriching column determines as needed；Externally there are two connect
Mouthful, it is respectively defined as interface X and interface Y；
The entrance of the sampling valve is connect with a port of two multiple-way valves, the outlet and liquid chromatography separation column battle array of sampling valve
The entrance of column connects, and the outlet of liquid chromatography separation column array is connect with detector；
By the state switching of two multiple-way valves of control, 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 two multiple-way valve packets
Include two ten-way valves, two eight ways valves and double two position four-way valves, including by multiple valve groups at and according to two ten-way valves or
Two eight ways valves or the valve group of double two position four-way valves principles operation are closed.
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| CN201910485296.3A CN110133162A (en) | 2019-05-27 | 2019-05-27 | Multidimensional liquid chromatographic separation system based on two multiple-way valves |
| PCT/CN2019/104868 WO2020052511A1 (en) | 2018-09-11 | 2019-09-09 | Multi-dimensional liquid chromatographic separation system |
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| CN201910485296.3A CN110133162A (en) | 2019-05-27 | 2019-05-27 | Multidimensional liquid chromatographic separation system based on two multiple-way valves |
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| CN110133162A true CN110133162A (en) | 2019-08-16 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020052511A1 (en) * | 2018-09-11 | 2020-03-19 | 李宜珊 | Multi-dimensional liquid chromatographic separation system |
| CN112611825A (en) * | 2020-12-30 | 2021-04-06 | 常州博世伟业生物科技有限公司 | Method and device for purifying plant polysaccharide by two-dimensional liquid chromatography |
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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 |
| CN109655561A (en) * | 2019-01-22 | 2019-04-19 | 李宜珊 | A kind of three-dimensional chromatographic fractionation system based on two ten-way valves |
| CN211043264U (en) * | 2019-05-27 | 2020-07-17 | 李宜珊 | Multidimensional liquid chromatography separation system based on two-position multi-way valve |
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2019
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN109655561A (en) * | 2019-01-22 | 2019-04-19 | 李宜珊 | A kind of three-dimensional chromatographic fractionation system based on two ten-way valves |
| CN211043264U (en) * | 2019-05-27 | 2020-07-17 | 李宜珊 | Multidimensional liquid chromatography separation system based on two-position multi-way valve |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020052511A1 (en) * | 2018-09-11 | 2020-03-19 | 李宜珊 | Multi-dimensional liquid chromatographic separation system |
| CN112611825A (en) * | 2020-12-30 | 2021-04-06 | 常州博世伟业生物科技有限公司 | Method and device for purifying plant polysaccharide by two-dimensional liquid chromatography |
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