CN116008416A - Liquid chromatograph - Google Patents
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- CN116008416A CN116008416A CN202211603020.9A CN202211603020A CN116008416A CN 116008416 A CN116008416 A CN 116008416A CN 202211603020 A CN202211603020 A CN 202211603020A CN 116008416 A CN116008416 A CN 116008416A
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Abstract
A liquid chromatograph relates to the technical field of detection instruments. The liquid chromatograph comprises a solvent management device, an infusion driving device, a sample injection device, a valve group device, a chromatographic separation device and a detection device which are connected in sequence; the chromatographic separation device comprises a plurality of chromatographic columns; the infusion driving device can drive the sample in the solvent management device to sequentially pass through the sample injection device, the valve group device and the chromatographic separation device and convey the sample to the detection device; the valve block assembly has different operating positions to allow samples from the sample introduction device to be loaded into one or more of the chromatographic columns in the chromatographic separation device for separation. The invention aims to provide a liquid chromatograph, which solves the technical problem that a single chromatographic column in the prior art needs to be replaced manually when analyzing a complex sample to a certain extent.
Description
Technical Field
The invention relates to the technical field of detection instruments, in particular to a liquid chromatograph.
Background
Liquid chromatography is an instrument that uses the difference in partition ratio of a mixture between a mobile phase and a stationary phase to separate the mixture first and then analyze and identify the mixture. The liquid chromatograph mainly comprises a sample injector, an infusion pump, a chromatographic column, a column temperature box and a detector which are connected by pipelines.
When analyzing complex samples, high performance liquid chromatography often encounters the situation that components and endogenous impurities are not easy to separate or are incompletely separated, so that a plurality of chromatographic columns are required to be connected in series/parallel, types of chromatographic columns used for different analysis components are different, and the analysis is also required to be switched. The existing liquid chromatograph is mostly provided with a single chromatographic column in a column incubator, an operator is required to manually replace the chromatographic column, the process is complicated, and risks such as leakage are easy to occur in the operation process.
Disclosure of Invention
The invention aims to provide a liquid chromatograph, which solves the technical problem that a single chromatographic column in the prior art needs to be replaced manually when analyzing a complex sample to a certain extent.
In order to achieve the above object, the present invention provides the following technical solutions:
a liquid chromatograph comprises a solvent management device, an infusion driving device, a sample injection device, a valve group device, a chromatographic separation device and a detection device which are connected in sequence;
the chromatographic separation device comprises a plurality of chromatographic columns;
the infusion driving device can drive the sample in the solvent management device to sequentially pass through the sample injection device, the valve group device and the chromatographic separation device and convey the sample to the detection device;
the valve block assembly has different operating positions to allow samples from the sample introduction device to be loaded into one or more of the chromatographic columns in the chromatographic separation device for separation.
In any of the above solutions, optionally, the valve group device includes a switching valve and a plurality of multi-way valves;
the switching valve comprises a switching input port and a plurality of switching output ports; the switching input port is communicated with the sample injection device;
part of the switching output ports are communicated with the corresponding chromatographic columns, and part of the switching output ports are communicated with the corresponding plurality of chromatographic columns through the multi-way valves;
the switching valve and the multi-way valve have different working positions so that the sample injection device is communicated with different chromatographic columns.
In any of the above aspects, optionally, the chromatography column comprises a pretreatment column; the pretreatment column comprises a corresponding pretreatment column first end and a pretreatment column second end; the first end of the pretreatment column and the second end of the pretreatment column are respectively communicated with different ports of the multi-way valve;
the multi-way valve also comprises a through hole communicated with the waste liquid device;
the switching output port comprises a switching pretreatment outlet communicated with the multi-way valve;
when the switching valve is in the pretreatment working position and the multi-way valve is in the pretreatment working position, the sample injection device is communicated with the first end of the pretreatment column, and the second end of the pretreatment column is communicated with the waste liquid device; when the switching valve is in the pretreatment working position, the switching input port is communicated with the switching pretreatment outlet.
In any of the above aspects, optionally, the chromatographic column further comprises an analytical column; the analytical column comprises a corresponding first analytical column end and a corresponding second analytical column end; the first end of the analysis column is communicated with the multi-way valve, and the second end of the analysis column is communicated with the detection device;
the switching output port comprises a switching recoil detection output port communicated with the multi-way valve;
when the switching valve is in a backflushing detection working position and the multi-way valve is in the backflushing detection working position, the sample injection device is communicated with the second end of the pretreatment column, and the first end of the pretreatment column is communicated with the first end of the analysis column; when the switching valve is positioned at the recoil detection working position, the switching input port is communicated with the switching recoil detection output port.
In any of the above solutions, optionally, the multi-way valve includes a second two-position multi-way valve;
the second two-position multi-way valve comprises at least six through ports; the first port of the second two-position multi-way valve is communicated with the switching pretreatment outlet, the second port of the second two-position multi-way valve is communicated with the first end of the pretreatment column, the third port of the second two-position multi-way valve is communicated with the analysis column, the fourth port of the second two-position multi-way valve is communicated with the switching recoil detection outlet, the fifth port of the second two-position multi-way valve is communicated with the second end of the pretreatment column, and the sixth port of the second two-position multi-way valve is communicated with the waste liquid device;
when the multi-way valve is in the pretreatment working position, the first port of the second two-position multi-way valve is communicated with the second port, the third port of the second two-position multi-way valve is communicated with the fourth port, and the fifth port of the second two-position multi-way valve is communicated with the sixth port;
when the multi-way valve is in a recoil detection working position, a first port of the second two-position multi-way valve is communicated with a sixth port, a second port of the second two-position multi-way valve is communicated with a third port, and a fourth port of the second two-position multi-way valve is communicated with a fifth port;
the second two-position multi-way valve is a two-position six-way valve;
the length of the pretreatment column is 3cm-5cm, and the particle size of the filler particles in the pretreatment column is 5 mu m-40 mu m.
In any of the above aspects, optionally, the chromatographic column comprises a third chromatographic column and a fourth chromatographic column; two ends of the third chromatographic column are respectively communicated with different ports of the multi-way valve;
the switching output port comprises a third switching outlet and a fourth switching outlet; the third switching outlet is communicated with the multi-way valve, the fourth switching outlet is communicated with one end of the fourth chromatographic column, and the other end of the fourth chromatographic column is communicated with the multi-way valve;
the sample injection device is communicated with the detection device through the third chromatographic column when the switching valve is positioned in the first working position and the switching input port is communicated with the third switching output port;
when the switching valve is positioned at the switching input port and is communicated with the fourth switching outlet, and when the multi-way valve is positioned at the second working position, the sample injection device is communicated with the detection device through the fourth chromatographic column and the third chromatographic column in sequence.
In any of the above solutions, optionally, the multi-way valve includes a first two-position multi-way valve;
the first two-position multi-way valve comprises at least six ports; the first port of the first two-position multi-way valve is communicated with the third switching outlet, the second port of the first two-position multi-way valve is communicated with the inlet end of the third chromatographic column, the third port of the first two-position multi-way valve is communicated with the outlet end of the fourth chromatographic column, the fourth port and the sixth port of the first two-position multi-way valve are both communicated with the detection device, and the fifth port of the first two-position multi-way valve is communicated with the outlet end of the third chromatographic column;
when the multi-way valve is in a first working position, a first port of the first two-position multi-way valve is communicated with a second port, a third port of the first two-position multi-way valve is communicated with a fourth port, and a fifth port of the first two-position multi-way valve is communicated with a sixth port;
when the multi-way valve is in the second working position, the first port of the first two-position multi-way valve is communicated with the sixth port, the second port of the first two-position multi-way valve is communicated with the third port, and the fourth port of the first two-position multi-way valve is communicated with the fifth port;
the first two-position multi-way valve is a two-position six-way valve.
In any of the foregoing aspects, optionally, the switch output comprises a first switch output, and the chromatographic column comprises a first chromatographic column; one end of the first chromatographic column is communicated with the first switching outlet, and the other end of the first chromatographic column is communicated with the detection device;
the switch output port further comprises a second switch output port, and the chromatographic column further comprises a second chromatographic column; one end of the second chromatographic column is communicated with the second switching outlet, and the other end of the second chromatographic column is communicated with the detection device.
In any of the above technical solutions, optionally, the chromatographic separation device further includes a column incubator, and the chromatographic column is disposed in the column incubator.
In any of the above solutions, optionally, the infusion driving device includes an infusion pump;
the sample injection device comprises a sample injector;
the switching valve is a one-to-six switching valve.
The beneficial effects of the invention are mainly as follows:
the liquid chromatograph provided by the invention comprises a plurality of chromatographic columns through the chromatographic separation device, and the valve group device has different working positions, so that the transfusion driving device drives the sample in the solvent management device to enter the sample injection device, and the sample is loaded into one or more chromatographic columns in the chromatographic separation device through the sample injection device to be separated and is transmitted to the detection device. When sample analysis is carried out, can be according to the complexity of sample, the different working positions of change valve group device select single chromatographic column or select a plurality of chromatographic column cooperation, do not need the manual replacement chromatographic column operation, simplified the operation process, also avoided the seepage risk that the manual replacement leads to a certain extent.
In order to make the above objects, features and advantages of the present application more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of a liquid chromatograph according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a switching valve according to an embodiment of the present invention;
fig. 3 is a schematic diagram of a first detection mode of a liquid chromatograph according to an embodiment of the present invention;
fig. 4 is a schematic diagram of a second detection mode of the liquid chromatograph according to the embodiment of the present invention;
fig. 5 is a schematic diagram of a third detection mode of a liquid chromatograph according to an embodiment of the present invention;
fig. 6 is a schematic diagram of a fourth detection mode of a liquid chromatograph according to an embodiment of the present invention;
fig. 7 is a schematic diagram of a fifth detection mode of the liquid chromatograph according to the embodiment of the present invention.
Icon: 100-solvent management device; 200-transfusion driving device; 300-sample injection device; 400-valve block arrangement; 410-a switching valve; 411-switching input ports; 412-switching the output port; 4121-a first switching outlet; 4122-a second switching outlet; 4123-a third switching outlet; 4124-fourth switching outlet; 4125-switching a pretreatment outlet; 4126-switching the recoil detection output port; 420-multiport valve; 421-first two-position multi-way valve; 422-a second two-position multi-way valve; 500-chromatographic separation device; 510-a first chromatographic column; 520-a second chromatographic column; 530-third chromatographic column; 540-fourth chromatographic column; 550-pretreatment column; 551-pretreatment column first end; 552-pretreatment column second end; 560-analytical column; 561-analytical column first end; 600-detecting device; 700-waste liquid device.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
In the description of the present invention, it should be noted that, directions or positional relationships indicated by terms such as "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., are directions or positional relationships based on those shown in the drawings, or are directions or positional relationships conventionally put in use of the inventive product, are merely for convenience of describing the present invention and simplifying the description, and are not indicative or implying that the apparatus or element to be referred to must have a specific direction, be constructed and operated in a specific direction, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used merely to distinguish between descriptions and should not be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal," "vertical," "overhang," and the like do not denote a requirement that the component be absolutely horizontal or overhang, but rather may be slightly inclined. As "horizontal" merely means that its direction is more horizontal than "vertical", and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present invention, it should also be noted that, unless explicitly specified and limited otherwise, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
Some embodiments of the present invention are described in detail below with reference to the accompanying drawings. The following embodiments and features of the embodiments may be combined with each other without conflict.
Examples
The present embodiment provides a liquid chromatograph; referring to fig. 1 to 7, fig. 1 is a schematic structural diagram of a liquid chromatograph provided in the present embodiment, and fig. 2 is a schematic structural diagram of a switching valve provided in the present embodiment; fig. 3 to fig. 7 are schematic diagrams of five detection modes of the liquid chromatograph provided in the present embodiment, wherein fig. 3 and fig. 4 are schematic diagrams of single chromatographic column detection, fig. 5 is a schematic diagram of serial detection of two chromatographic columns, fig. 6 is a schematic diagram of sample pretreatment enrichment, and fig. 7 is a schematic diagram of backflushing analysis detection. Wherein the solid lines and arrows in fig. 4-7 are the direction of sample flow.
Referring to fig. 1 to 7, the liquid chromatograph provided in this embodiment includes a solvent management device 100, an infusion driving device 200, a sample injection device 300, a valve group device 400, a chromatographic separation device 500, and a detection device 600, which are sequentially connected. Optionally, the infusion drive device 200 comprises an infusion pump. Optionally, the sample introduction device 300 comprises a sample injector. Alternatively, the switching valve is a one-to-six switching valve or other switching valve.
The chromatographic separation device 500 includes a plurality of chromatographic columns; optionally, the chromatographic separation device 500 further comprises a column incubator within which the chromatographic column is disposed.
The infusion driving device 200 can drive the sample in the solvent management device 100 to sequentially pass through the sample injection device 300, the valve group device 400 and the chromatographic separation device 500, and convey the sample to the detection device 600. Wherein the sample within the solvent management device 100 is a mobile phase.
The valve block assembly 400 has different operating positions to allow samples from the sample introduction device 300 to be loaded into one or more chromatographic columns in the chromatographic separation device 500 for separation.
In the liquid chromatograph of the present embodiment, the chromatographic separation device 500 includes a plurality of chromatographic columns, and the valve assembly 400 has different working positions, so that the infusion driving device 200 drives the sample in the solvent management device 100 to enter the sample injection device 300, and the sample is loaded into one or more chromatographic columns in the chromatographic separation device 500 through the sample injection device 300 for separation, and is delivered to the detection device 600. When sample analysis is performed, according to the complexity of the sample, different working positions of the valve bank device 400 can be switched, and a single chromatographic column or a plurality of chromatographic columns can be selected for matching, so that the operation of manually replacing the chromatographic columns is not needed, the operation process is simplified, and the leakage risk caused by manual replacement is avoided to a certain extent.
Referring to fig. 1-7, in an alternative version of this embodiment, a valve block assembly 400 includes a switching valve 410 and a plurality of multi-way valves 420. The switching valve 410 and the multi-way valve 420 are matched to provide a foundation for high-efficiency liquid-phase color complex sample analysis such as chromatographic column switching, chromatographic column serial connection, sample pretreatment enrichment, backflushing analysis detection and the like.
Optionally, the switching valve 410 comprises a switching input 411 and several switching output 412; the switching input 411 communicates with the sample injection device 300.
The partial switching output ports 412 are communicated with corresponding chromatographic columns, and the partial switching output ports 412 are communicated with corresponding plurality of chromatographic columns through the multi-way valves 420; it will be appreciated that the switch output 412 may be in direct communication with a corresponding column or may be in communication with a corresponding number of columns through the multi-way valve 420.
The switching valve 410 and the multi-way valve 420 have different operating positions to allow the sample injection device 300 to communicate with different chromatographic columns. The multi-way valve 420 is switched to different working positions by the switching valve 410, so that the sample injection device 300 is communicated with different chromatographic columns, and high performance liquid color complex sample analysis such as chromatographic column switching, chromatographic column serial connection, sample pretreatment enrichment, backflushing analysis detection and the like can be realized.
Referring to fig. 1, 6 and 7, in an alternative to this embodiment, the chromatographic column comprises a pretreatment column 550; the pretreatment column 550 includes a corresponding pretreatment column first end 551 and pretreatment column second end 552; the pretreatment column first end 551 and the pretreatment column second end 552 are each in communication with a different port of the multi-port valve 420.
The multi-way valve 420 also includes a port that communicates with the waste device 700.
The switch output 412 of the switch valve 410 includes a switch preconditioning outlet 4125 in communication with the multi-way valve 420.
Alternatively, as shown in fig. 6, when the switching valve 410 is in the pretreatment operating position and the multi-way valve 420 is in the pretreatment operating position, the sample injection device 300 is communicated with the first end 551 of the pretreatment column, and the second end 552 of the pretreatment column is communicated with the waste liquid device 700; wherein, when the switching valve 410 is in the pretreatment operation position, the switching input port 411 is communicated with the switching pretreatment outlet 4125. By the switching valve 410 being in the pretreatment operating position and the multi-way valve 420 being in the pretreatment operating position, the components to be tested in the sample in the solvent management device 100 can be retained on the column head of the pretreatment column 550, and most of the impurities flow into the waste liquid device 700 through the second end 552 of the pretreatment column, so as to achieve the purposes of purifying and enriching the sample.
Referring to fig. 1, 6 and 7, in an alternative to this embodiment, the chromatographic column further comprises an analytical column 560; analytical column 560 includes a corresponding analytical column first end 561 and analytical column second end; the analytical column first end 561 communicates with the multi-way valve 420 and the analytical column second end communicates with the detection device 600.
The switch output 412 of the switch valve 410 includes a switch kick-back detection output 4126 in communication with the multi-way valve 420.
Alternatively, as shown in fig. 7, when the switching valve 410 is in the back flush detection operating position and the multi-way valve 420 is in the back flush detection operating position, the sample injection device 300 is in communication with the pretreatment column second end 552, and the pretreatment column first end 551 is in communication with the analysis column first end 561; when the switching valve 410 is in the recoil detection operation position, the switching input port 411 communicates with the switching recoil detection output port 4126.
Referring to fig. 1, 6 and 7, in an alternative to this embodiment, the multi-way valve 420 includes a second two-position multi-way valve 422.
The second two-position multi-way valve 422 includes at least six ports; for example, the first port of the second two-way multi-way valve 422 communicates with the switching pretreatment outlet 4125 of the switching valve 410, the second port of the second two-way multi-way valve 422 communicates with the pretreatment column first end 551, the third port of the second two-way multi-way valve 422 communicates with the analytical column first end 561 of the analytical column 560, the fourth port of the second two-way multi-way valve 422 communicates with the switching recoil detection outlet 4126 of the switching valve 410, the fifth port of the second two-way multi-way valve 422 communicates with the pretreatment column second end 552, and the sixth port of the second two-way multi-way valve 422 communicates with the waste device 700; as shown in fig. 6 and 7, the first through sixth ports of the second two-position multi-way valve 422 correspond to 1-6 in the second two-position multi-way valve 422, respectively.
Alternatively, as shown in fig. 1 and 6, when the multi-way valve 420 is in the pretreatment operation position, the first port of the second two-position multi-way valve 422 is communicated with the second port, the third port of the second two-position multi-way valve 422 is communicated with the fourth port, and the fifth port of the second two-position multi-way valve 422 is communicated with the sixth port. For example, when the switching valve 410 is in the pretreatment operation position and the multi-way valve 420 is in the pretreatment operation position, the switching input port 411 is communicated with the switching pretreatment outlet 4125, the sample from the sample injection device 300 sequentially passes through the switching input port 411, the switching pretreatment outlet 4125, the first port of the second two-way multi-way valve 422 and the second port of the second two-way multi-way valve 422, the component to be tested in the sample is retained on the column head of the pretreatment column 550 through the first end 551 of the pretreatment column, and most of the impurities sequentially flow into the waste liquid device 700 through the second end 552 of the pretreatment column, the fifth port of the second two-way multi-way valve 422 and the sixth port of the second two-way multi-way valve 422, so as to achieve the purposes of purifying and enriching the sample.
Alternatively, as shown in fig. 1 and 7, when the multi-way valve 420 is in the recoil detection working position, the first port of the second two-position multi-way valve 422 is communicated with the sixth port, the second port of the second two-position multi-way valve 422 is communicated with the third port, and the fourth port of the second two-position multi-way valve 422 is communicated with the fifth port; for example, when the switching valve 410 is in the back flush detection operating position and the multi-way valve 420 is in the back flush detection operating position, the switching input port 411 is in communication with the switching back flush detection output port 4126, and the sample from the sample injection device 300 sequentially passes through the switching input port 411, the switching back flush detection output port 4126, the fourth port of the second two-way multi-way valve 422, and the fifth port of the second two-way multi-way valve 422, and the component to be tested remaining on the column head of the pretreatment column 550 sequentially passes through the first end 551 of the pretreatment column, the second port of the second two-way multi-way valve 422, and the third port of the second two-way multi-way valve 422, and then enters the analysis column 560 and the detection device 600 for separation and measurement.
In this embodiment, after the components to be tested in the sample in the solvent management apparatus 100 are purified and enriched by the pretreatment column 550, the pretreatment is finished; then the switching valve 410 is switched from the pretreatment working position to the backflushing detection working position, that is, the pretreatment outlet 4125 is switched to the backflushing detection outlet 4126, the second two-position multi-way valve 422 is switched from the pretreatment working position to the backflushing detection working position, the components to be detected remained on the column head of the pretreatment column 550 are backflushed and enter the analysis column 560 and the detection device 600 for separation and measurement, after a period of time, the switching valve 410 is switched to the pretreatment working position again, the pretreatment column 550 is subjected to regeneration treatment, and the next sample injection is waited.
In this embodiment, the pretreatment column 550 is not too long, and the length of the pretreatment column 550 is usually 3cm to 5cm, and the particle size of the filler particles in the pretreatment column 550 is 5 μm to 40. Mu.m. However, if the biological sample is directly taken for injection, the particle size of the filler particles needs to be increased; and a pretreatment column sieve plate with larger aperture, such as 40 μm, is selected. The coarse-particle size packing and the large-pore sieve plates are selected to prevent clogging with macromolecular impurities and to extend the life of the pretreatment column 550. In addition, before and after each sample injection, the sample injection device 300 and the pretreatment column 550 are usually cleaned by adopting a proper cleaning solution to eliminate the interference of the residues on the next measurement and prolong the service life of the pretreatment column 550. The manner of column switching can be divided into two types according to whether the flow direction of the analytical mobile phase and the pretreatment mobile phase are the same or not: forward flushing and back flushing. In the backflush mode, the direction of the switched analytical mobile phase entering the pretreatment column 550 is opposite to the direction of the pretreated mobile phase. Otherwise, the process is forward.
In this embodiment, the switching mode, pretreatment time and switching time of the switching valve 410 and the multi-way valve 420 depend on the retention of the tested components on the pretreatment column, and the principle is to achieve short analysis time, good separation and high recovery rate.
Optionally, the second two-position multi-way valve 422 is a two-position six-way valve. The second two-position multi-way valve 422 includes six ports. In this embodiment, the second two-position multi-way valve 422 may be another valve.
Referring to fig. 1, 4 and 5, in an alternative of the present embodiment, the chromatographic column includes a third chromatographic column 530 and a fourth chromatographic column 540; the two ends of the third chromatographic column 530 are respectively communicated with different ports of the multi-port valve 420.
The switching output 412 of the switching valve 410 includes a third switching outlet 4123 and a fourth switching outlet 4124; the third switching outlet 4123 communicates with the multi-way valve 420, the fourth switching outlet 4124 communicates with one end of the fourth chromatographic column 540, and the other end of the fourth chromatographic column 540 communicates with the multi-way valve 420; for example, the inlet end of the fourth chromatographic column 540 communicates with the fourth switching outlet 4124 of the switching valve 410 and the outlet end of the fourth chromatographic column 540 communicates with the multi-way valve 420.
Alternatively, as shown in fig. 4, when the switching valve 410 is in communication with the switching input 411 and the third switching output 4123, and the multi-way valve 420 is in the first working position, the sample injection device 300 is in communication with the detection device 600 through the third chromatographic column 530.
Alternatively, as shown in fig. 5, when the switching valve 410 is in communication with the switching input 411 and the fourth switching output 4124, and the multi-way valve 420 is in the second working position, the sample injection device 300 is sequentially connected to the detection device 600 through the fourth chromatographic column 540 and the third chromatographic column 530.
Referring to fig. 1, 4 and 5, in an alternative to this embodiment, the multi-way valve 420 includes a first two-position multi-way valve 421.
The first two-position multi-way valve 421 includes at least six ports; for example, the first port of the first two-way multi-port valve 421 is communicated with the third switching outlet 4123 of the switching valve 410, the second port of the first two-way multi-port valve 421 is communicated with the inlet end of the third chromatographic column 530, the third port of the first two-way multi-port valve 421 is communicated with the outlet end of the fourth chromatographic column 540, the fourth port and the sixth port of the first two-way multi-port valve 421 are both communicated with the detection device 600, and the fifth port of the first two-way multi-port valve 421 is communicated with the outlet end of the third chromatographic column 530; as shown in fig. 4 and 5, the first through sixth ports of the first two-position multi-way valve 421 correspond to 1-6 in the first two-position multi-way valve 421 in the drawings, respectively.
Alternatively, as shown in fig. 1 and 4, when the multi-way valve 420 is in the first working position, the first port of the first two-position multi-way valve 421 is communicated with the second port, the third port of the first two-position multi-way valve 421 is communicated with the fourth port, and the fifth port of the first two-position multi-way valve 421 is communicated with the sixth port; for example, when the switching valve 410 is in communication with the switching input 411 and the third switching output 4123, and the multi-way valve 420 is in the first operating position, the sample from the sample injection device 300 sequentially passes through the switching input 411, the third switching output 4123, the first port of the first two-way multi-way valve 421, the second port of the first two-way multi-way valve 421, the third chromatography column 530, the fifth port of the first two-way multi-way valve 421, and the sixth port of the first two-way multi-way valve 421, and enters the detection device 600.
Alternatively, as shown in fig. 1 and 5, when the multi-way valve 420 is in the second working position, the first port of the first two-position multi-way valve 421 is communicated with the sixth port, the second port of the first two-position multi-way valve 421 is communicated with the third port, and the fourth port of the first two-position multi-way valve 421 is communicated with the fifth port; for example, when the switching valve 410 is in communication with the switching input 411 and the fourth switching output 4124, and the multi-way valve 420 is in the second operating position, the sample from the sample injection device 300 sequentially passes through the switching input 411, the fourth switching output 4124, the fourth chromatographic column 540, the third port of the first two-position multi-way valve 421, the second port of the first two-position multi-way valve 421, the third chromatographic column 530, the fifth port of the first two-position multi-way valve 421, and the fourth port of the first two-position multi-way valve 421, and enters the detection device 600.
In this embodiment, multiple columns are required to be connected in series for detection of complex samples. For example, when the spectrum of the sample separated by the third chromatographic column 530 is found to be not ideal, the plurality of peaks are not separated, the fourth chromatographic column 540 capable of separating can be selected according to the properties of the components which are not separated, the switching valve 410 connected to fig. 5 is positioned at the switching input 411 and is communicated with the fourth switching output 4124, the multi-way valve 420 is positioned at the second working position, the fourth chromatographic column 540 and the third chromatographic column 530 are used in series, and the sample enters the detection device 600 after passing through the two chromatographic columns, so as to realize separation detection of the components which are difficult to separate by the single chromatographic column.
Alternatively, the first two-position multi-way valve 421 is a two-position six-way valve. The first two-position multi-way valve 421 includes six ports. In this embodiment, the first two-position multi-way valve 421 may be another valve.
Referring to fig. 1-3, in an alternative version of the present embodiment, the switch output 412 of the switch valve 410 comprises a first switch output 4121, and the chromatographic column comprises a first chromatographic column 510; one end of the first chromatographic column 510 is communicated with the first switching outlet 4121, and the other end of the first chromatographic column 510 is communicated with the detection device 600 to realize the application of a single chromatographic column.
Referring to fig. 1-3, in an alternative version of the present embodiment, the switch output 412 of the switch valve 410 further comprises a second switch outlet 4122, and the chromatographic column further comprises a second chromatographic column 520; one end of the second chromatographic column 520 is in communication with the second switching outlet 4122 and the other end of the second chromatographic column 520 is in communication with the detection device 600. When different sample detection is performed through the first switching outlet 4121, the second switching outlet 4122, the first chromatographic column 510 and the second chromatographic column 520, the chromatographic column can be switched through automatic switching of the first switching outlet 4121 and the second switching outlet 4122, and then the chromatographic column enters the detection device 600, so that automatic switching of the chromatographic column is realized. In this embodiment, other numbers, such as 3, 5, etc., may be used for a single column.
The liquid chromatograph in the embodiment can automatically realize chromatographic column switching, chromatographic column serial connection, sample pretreatment enrichment and recoil analysis detection; the automatic switching of a plurality of single chromatographic columns can be realized through the form of valves 400 automatic switch, the repeated switch of a column incubator (the temperature in the column incubator is kept constant, once the column incubator is opened, the stable temperature is recovered for a long time, the relevant detection can not be carried out in the period of time), the manual replacement of the chromatographic columns by an experimenter (the two ends of the chromatographic columns are connected with a pipeline by using special threads, the threads at the two ends are required to be opened during the replacement, the new chromatographic columns are connected later, and the connected pipeline is required to be ensured not to leak liquid) can be avoided, the operation difficulty of experimenters is reduced to a certain extent, and the liquid leakage risk is reduced.
The liquid chromatograph in this embodiment also realizes the series connection of a plurality of chromatographic columns of automatic switch-over, can realize a plurality of chromatographic columns separation of complicated component, and for current single chromatographic column, detection device application scope is wider, and detection accuracy is higher.
The liquid chromatograph also has pretreatment and backflushing technology and has the advantages of (1) online purification, simple pretreatment and automatic operation; the sample can be directly sampled and measured by simple treatment. (2) The method enriches the components to be detected, improves the analysis sensitivity, and is particularly suitable for components which are difficult to purify and are enriched and have larger polarity.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The liquid chromatograph is characterized by comprising a solvent management device, an infusion driving device, a sample injection device, a valve group device, a chromatographic separation device and a detection device which are connected in sequence;
the chromatographic separation device comprises a plurality of chromatographic columns;
the infusion driving device can drive the sample in the solvent management device to sequentially pass through the sample injection device, the valve group device and the chromatographic separation device and convey the sample to the detection device;
the valve block assembly has different operating positions to allow samples from the sample introduction device to be loaded into one or more of the chromatographic columns in the chromatographic separation device for separation.
2. The liquid chromatograph of claim 1, wherein the valve assembly comprises a switching valve and a plurality of multi-way valves;
the switching valve comprises a switching input port and a plurality of switching output ports; the switching input port is communicated with the sample injection device;
part of the switching output ports are communicated with the corresponding chromatographic columns, and part of the switching output ports are communicated with the corresponding plurality of chromatographic columns through the multi-way valves;
the switching valve and the multi-way valve have different working positions so that the sample injection device is communicated with different chromatographic columns.
3. The liquid chromatograph of claim 2, wherein the chromatographic column comprises a pretreatment column; the pretreatment column comprises a corresponding pretreatment column first end and a pretreatment column second end; the first end of the pretreatment column and the second end of the pretreatment column are respectively communicated with different ports of the multi-way valve;
the multi-way valve also comprises a through hole communicated with the waste liquid device;
the switching output port comprises a switching pretreatment outlet communicated with the multi-way valve;
when the switching valve is in the pretreatment working position and the multi-way valve is in the pretreatment working position, the sample injection device is communicated with the first end of the pretreatment column, and the second end of the pretreatment column is communicated with the waste liquid device; when the switching valve is in the pretreatment working position, the switching input port is communicated with the switching pretreatment outlet.
4. The liquid chromatograph of claim 3, wherein the chromatographic column further comprises an analytical column; the analytical column comprises a corresponding first analytical column end and a corresponding second analytical column end; the first end of the analysis column is communicated with the multi-way valve, and the second end of the analysis column is communicated with the detection device;
the switching output port comprises a switching recoil detection output port communicated with the multi-way valve;
when the switching valve is in a backflushing detection working position and the multi-way valve is in the backflushing detection working position, the sample injection device is communicated with the second end of the pretreatment column, and the first end of the pretreatment column is communicated with the first end of the analysis column; when the switching valve is positioned at the recoil detection working position, the switching input port is communicated with the switching recoil detection output port.
5. The liquid chromatograph of claim 4, wherein the multi-way valve comprises a second two-position multi-way valve;
the second two-position multi-way valve comprises at least six through ports; the first port of the second two-position multi-way valve is communicated with the switching pretreatment outlet, the second port of the second two-position multi-way valve is communicated with the first end of the pretreatment column, the third port of the second two-position multi-way valve is communicated with the analysis column, the fourth port of the second two-position multi-way valve is communicated with the switching recoil detection outlet, the fifth port of the second two-position multi-way valve is communicated with the second end of the pretreatment column, and the sixth port of the second two-position multi-way valve is communicated with the waste liquid device;
when the multi-way valve is in the pretreatment working position, the first port of the second two-position multi-way valve is communicated with the second port, the third port of the second two-position multi-way valve is communicated with the fourth port, and the fifth port of the second two-position multi-way valve is communicated with the sixth port;
when the multi-way valve is in a recoil detection working position, a first port of the second two-position multi-way valve is communicated with a sixth port, a second port of the second two-position multi-way valve is communicated with a third port, and a fourth port of the second two-position multi-way valve is communicated with a fifth port;
the second two-position multi-way valve is a two-position six-way valve;
the length of the pretreatment column is 3cm-5cm, and the particle size of the filler particles in the pretreatment column is 5 mu m-40 mu m.
6. The liquid chromatograph of claim 2, wherein the chromatographic column comprises a third chromatographic column and a fourth chromatographic column; two ends of the third chromatographic column are respectively communicated with different ports of the multi-way valve;
the switching output port comprises a third switching outlet and a fourth switching outlet; the third switching outlet is communicated with the multi-way valve, the fourth switching outlet is communicated with one end of the fourth chromatographic column, and the other end of the fourth chromatographic column is communicated with the multi-way valve;
the sample injection device is communicated with the detection device through the third chromatographic column when the switching valve is positioned in the first working position and the switching input port is communicated with the third switching output port;
when the switching valve is positioned at the switching input port and is communicated with the fourth switching outlet, and when the multi-way valve is positioned at the second working position, the sample injection device is communicated with the detection device through the fourth chromatographic column and the third chromatographic column in sequence.
7. The liquid chromatograph of claim 6, wherein the multi-way valve comprises a first two-position multi-way valve;
the first two-position multi-way valve comprises at least six ports; the first port of the first two-position multi-way valve is communicated with the third switching outlet, the second port of the first two-position multi-way valve is communicated with the inlet end of the third chromatographic column, the third port of the first two-position multi-way valve is communicated with the outlet end of the fourth chromatographic column, the fourth port and the sixth port of the first two-position multi-way valve are both communicated with the detection device, and the fifth port of the first two-position multi-way valve is communicated with the outlet end of the third chromatographic column;
when the multi-way valve is in a first working position, a first port of the first two-position multi-way valve is communicated with a second port, a third port of the first two-position multi-way valve is communicated with a fourth port, and a fifth port of the first two-position multi-way valve is communicated with a sixth port;
when the multi-way valve is in the second working position, the first port of the first two-position multi-way valve is communicated with the sixth port, the second port of the first two-position multi-way valve is communicated with the third port, and the fourth port of the first two-position multi-way valve is communicated with the fifth port;
the first two-position multi-way valve is a two-position six-way valve.
8. The liquid chromatograph of claim 2, wherein the switch output comprises a first switch output and the chromatographic column comprises a first chromatographic column; one end of the first chromatographic column is communicated with the first switching outlet, and the other end of the first chromatographic column is communicated with the detection device;
the switch output port further comprises a second switch output port, and the chromatographic column further comprises a second chromatographic column; one end of the second chromatographic column is communicated with the second switching outlet, and the other end of the second chromatographic column is communicated with the detection device.
9. The liquid chromatograph of claim 1, wherein the chromatographic separation device further comprises a column oven, the chromatographic column being disposed within the column oven.
10. The liquid chromatograph of claim 2, wherein the infusion drive device comprises an infusion pump;
the sample injection device comprises a sample injector;
the switching valve is a one-to-six switching valve.
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| CN202211603020.9A CN116008416A (en) | 2022-12-13 | 2022-12-13 | Liquid chromatograph |
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| CN202211603020.9A CN116008416A (en) | 2022-12-13 | 2022-12-13 | Liquid chromatograph |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117130297A (en) * | 2023-10-25 | 2023-11-28 | 北京豪思生物科技股份有限公司 | Upper computer control method, device and equipment of liquid chromatograph |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117130297A (en) * | 2023-10-25 | 2023-11-28 | 北京豪思生物科技股份有限公司 | Upper computer control method, device and equipment of liquid chromatograph |
| CN117130297B (en) * | 2023-10-25 | 2023-12-29 | 北京豪思生物科技股份有限公司 | Upper computer control method, device and equipment of liquid chromatograph |
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