A column selection valve, a sample injection chromatography device and a sample injection control method thereof
By designing a column selection valve for liquid chromatography experiments, the bypass, loading and flushing of the chromatography columns is achieved, solving the problems of cumbersome disassembly of chromatography columns and insufficient pressure sensing protection in the prior art, and improving the experimental efficiency and column protection effect.
Patent Information
- Application Number
- CN202110147933.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2021-02-03
- Publication Date
- 2025-04-08
- Estimated Expiration
- 2041-02-03
AI Technical Summary
In existing liquid chromatography experiments, the disassembly and replacement of the chromatographic column is cumbersome, which can easily lead to damage to the column performance. The existing system lacks effective pressure sensing protection and cannot monitor and prevent overpressure in real time.
A column selection valve is designed, including the valve body and the valve core, bypassing, forward upward and reverse flushing of the column through the through grooves on the valve core, reducing the need for physical disassembly of the column and adding a pressure sensor to monitor and prevent overpressure.
The efficient bypass, loading and rinsing of the chromatography column is achieved, reducing experimental time and labor costs, improving experimental efficiency and convenience, and protecting the chromatography column through real-time pressure monitoring.
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Figure CN112986464B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of chromatography devices, and in particular to a column selection valve, a sample injection chromatography device and a sample injection control method thereof. Background Art
[0002] In liquid chromatography experiments, after finishing a column, the staff needs to remove it and replace it with another column before proceeding to the next experiment. There are many disadvantages in this process, such as the need to frequently remove the column from the chromatography system. When removing the column, it is often easy for a small amount of bubbles to enter the column due to unskilled operation or accidental factors, affecting the performance and use of the column. Even if the bubbles can be discharged from the column, the process is very time-consuming and laborious.
[0003] At present, existing instruments use the method of three columns in parallel. In the preparation stage before the experiment, the chromatography columns are flushed online, and there is no need to replace and flush them again during the experiment. This has good process development continuity and convenience, greatly improving the efficiency and convenience of the experiment. Figure 1 As shown, it includes a system pump 1', a loading valve 2', a sample pump 3', a column flow control valve 4', a first column selection valve 5', a second column selection valve 7', three chromatography columns 8' and a detector 9'. The outlet of the system pump 1' is connected to the buffer inlet of the loading valve 2', the outlet of the sample pump 3' is connected to the sample inlet of the loading valve 2', the column position valve 4' is a three-position four-way valve, the column position valve 4' is connected to the loading valve 2', the interface 1 and the interface 6 of the column position valve 4' are respectively connected to the first column selection valve 5' and the second column selection valve 7', the interface 2 of the column position valve 4' is connected to the detector 9', the interfaces corresponding to the first column selection valve 5' and the second column selection valve 7' are respectively connected through more than three chromatography columns 8', and at least one group of corresponding interfaces are directly connected through pipelines. However, this design still has many shortcomings:
[0004] (1) This system uses a column position valve and two column selection valves, which greatly increases the cost;
[0005] (2) The existing three-column position valve can improve the flushing efficiency, effectively protect the chromatography column, and leave a bypass flushing pipeline, which can also reduce the risk of column disassembly. However, when two column selection valves plus a column position valve are used to achieve these functions, more pipelines are needed to connect different valves, which increases the extra-column volume of the pipeline. Compared with a single valve, the efficiency of achieving these functions is lower;
[0006] (3) The existing system has only one pressure sensor, which detects the system pressure online and can protect the chromatography column. However, due to the lack of a second pressure sensor after the column, the pressure difference loaded on the chromatography packing cannot be measured, so the overpressure alarm cannot be set in real time, but the packing cannot be protected from overpressure. The defect of this device is that two column selection valves are required. The connection between a certain chromatography column and the respective column selection holes on the two column selection valves must follow a certain arrangement rule. This rule is generally controlled by software and is difficult to change after it is determined. When switching between chromatography columns or between chromatography columns and direct connections, the software must control the two column selection valve rotors to rotate simultaneously so that the respective column selection slots are connected to the corresponding column selection hole direct connection holes almost at the same time. This process has high synchronization and accuracy requirements, the software program is relatively complex, and the fault tolerance rate is low.
[0007] Therefore, in order to solve the above-mentioned technical problems, a column selection valve, an injection chromatography device and an injection control method thereof are now needed. Summary of the invention
[0008] In order to overcome the shortcomings of the prior art, the present invention provides a column selection valve, a sample injection chromatography device and a sample injection control method thereof, which can realize column bypass, forward loading and reverse flushing without frequently removing the chromatography column from the chromatography system, greatly improving the efficiency and convenience of the experiment. The technical solution is as follows:
[0009] In one aspect, the present invention provides a column selection valve for chromatography column switching control, comprising:
[0010] A valve body, wherein the valve body is provided with a loading valve interface connected to an external loading valve, a detector interface connected to an external detector, and a plurality of column interfaces connected to an external chromatography column, and the loading valve interface is controllably connected to one of the column interfaces;
[0011] A valve core, wherein at least one through groove is provided on the upper surface of the valve core, the valve core is arranged on the valve body, and can rotate relative to the valve body under the drive of the driving mechanism, and the through groove is used to connect the detector interface with another column interface.
[0012] Furthermore, the valve body is disc-shaped, the loading valve interface is arranged at the center of the valve body, and the detector interface, the plurality of column interfaces and the loading valve interface are equidistant from each other.
[0013] Furthermore, the number of the detector interfaces is two, and the two detector interfaces are connected to the detector via a two-inlet-one-outlet tee, and the loading valve interface can be connected to one of the column interfaces or one of the detector interfaces.
[0014] Furthermore, the through groove on the valve core is used to connect the detector interface with another column interface adjacent to it, and / or, the through groove is used to connect the detector interface with another column interface separated from it, and / or, the through groove is used to connect the loading valve interface with the detector interface and one of the multiple column interfaces.
[0015] Furthermore, the number of the through slots is four.
[0016] On the other hand, the present invention provides a sample injection chromatography device, comprising a plurality of chromatography columns and the column selection valve as described above, wherein both ends of the chromatography columns are respectively connected to the column interfaces on the valve body of the column selection valve in a one-to-one correspondence.
[0017] Furthermore, the sample introduction chromatography device further comprises a controller and a driving mechanism, wherein the controller is used to control the sample introduction valve interface of the column selection valve to communicate with one of the column interfaces or the detector interface;
[0018] Under the control of the controller, the driving mechanism drives the valve core of the column selection valve to rotate relative to the valve body.
[0019] Further, the chromatography column comprises a first chromatography column, a second chromatography column and a third chromatography column, and the column interface comprises a first positive column interface, a first negative column interface, a second positive column interface, a second negative column interface, a third positive column interface and a third negative column interface;
[0020] The first positive column interface, the second positive column interface, and the third positive column interface correspond to the injection ends of the first chromatography column, the second chromatography column, and the third chromatography column, respectively; the first negative column interface, the second negative column interface, and the third negative column interface correspond to the sample outlet ends of the first chromatography column, the second chromatography column, and the third chromatography column, respectively.
[0021] In another aspect, the present invention provides a method for controlling the injection of a sample into a chromatographic device, wherein the method controls the loading and / or backwashing of any chromatographic column in the chromatographic device.
[0022] Preliminarily connect the injection end of the target chromatography column to the interface of the target positive column, and connect the output end of the target chromatography column to the interface of the target negative column;
[0023] The sample loading control method comprises: controlling the sample loading valve interface of the column selection valve to be connected with the target positive column interface, controlling the valve core of the column selection valve to rotate until the target negative column interface is connected with the detector interface through the through groove on the valve core; and then opening the sample loading valve to load the sample;
[0024] The backwash control method includes: controlling the loading valve interface of the column selection valve to communicate with the target negative column interface, controlling the valve core to rotate until the target positive column interface and the detector interface are connected through the through groove on the valve core; and then opening the loading valve for backwashing.
[0025] Further, the column selection valve of the sample injection chromatography device includes a positive detector interface and a negative detector interface, characterized in that the control method also includes controlling the mobile phase bypass, including:
[0026] The positive detector interface and the negative detector interface are controlled to be connected to the detector through a three-way joint; and the loading valve interface of the column selection valve is controlled to be connected to the positive detector interface or the negative detector interface.
[0027] The beneficial effects brought by the technical solution provided by the present invention are as follows:
[0028] a. Use one column selection valve instead of multiple valves to avoid errors caused by asynchronous switching of multiple valves;
[0029] b. No need to flush or replace the chromatography column during the experiment, which has good process continuity and greatly improves the efficiency of the experiment;
[0030] c. Adding a three-column position valve can realize column bypass, forward loading and reverse flushing, which enhances the convenience of column operation. At the same time, the control logic of the column selection valve is simple, highly stable and not prone to errors;
[0031] d. By setting up a pressure sensor, the pressure difference loaded on the chromatography filler can be measured, so as to provide real-time overpressure prompts to achieve overpressure protection for the filler. BRIEF DESCRIPTION OF THE DRAWINGS
[0032] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.
[0033] Figure 1 It is a connection diagram of each component in the three-column parallel method in the prior art;
[0034] Figure 2 is a structural diagram of a valve body provided by an embodiment of the present invention;
[0035] Figure 3 is a structural diagram of a valve core provided by an embodiment of the present invention;
[0036] Figure 4 is a schematic diagram of a first working position provided by an embodiment of the present invention;
[0037] Figure 5 is a schematic diagram of a second working position provided by an embodiment of the present invention;
[0038] Figure 6is a schematic diagram of a third working position provided by an embodiment of the present invention;
[0039] Figure 7 is a schematic diagram of a fourth working position provided by an embodiment of the present invention;
[0040] Figure 8 is a schematic diagram of a fifth working position provided by an embodiment of the present invention;
[0041] Fig. 9 is a schematic diagram of a sixth working position provided by an embodiment of the present invention;
[0042] Fig.10 is a schematic diagram of a seventh working position provided by an embodiment of the present invention;
[0043] Fig.11 It is a schematic diagram of the eighth working position provided by an embodiment of the present invention.
[0044] Among them, the figure marks include: 1-valve body, 2-valve core, 11-sample valve interface. DETAILED DESCRIPTION
[0045] In order to enable those skilled in the art to better understand the scheme of the present invention, and to more clearly understand the purpose, technical scheme and advantages of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described below in conjunction with specific embodiments and with reference to the accompanying drawings. It should be noted that the implementation methods not shown or described in the accompanying drawings are forms known to those skilled in the art. In addition, although demonstrations of parameters containing specific values may be provided herein, it should be understood that the parameters do not need to be exactly equal to the corresponding values, but may be approximated to the corresponding values within an acceptable error tolerance or design constraint. Obviously, the described embodiments are only embodiments of a part of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative work should belong to the scope of protection of the present invention. In addition, the terms "including" and "having" in the specification and claims of the present invention and any of their variations are intended to cover non-exclusive inclusions, for example, a process, method, device, product or equipment containing a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or equipment.
[0046] In one embodiment of the present invention, a column selection valve for chromatography column switching control is provided, comprising a valve body and a valve core, such as Figure 2As shown, the valve body 1 is provided with a loading valve interface 11 connected to an external loading valve, a detector interface connected to an external detector, and multiple column interfaces connected to an external chromatography column, and the loading valve interface 11 can be communicated with one of the column interfaces or one of the detector interfaces. Figure 3 As shown, at least one through groove is provided on the upper surface of the valve core 2, the valve core 2 is arranged on the valve body 1, and can rotate relative to the valve body 1 under the drive of the driving mechanism, and the through groove is used to connect the detector interface with another column interface. There are two detector interfaces, and the two detector interfaces are connected to the detector through a two-input and one-output tee.
[0047] In one embodiment of the present invention, a sample injection chromatography device is provided, comprising a column selection valve as described above, a plurality of chromatography columns, a controller and a driving mechanism. The two ends of the chromatography column are respectively connected to the column interfaces on the valve body 1 of the column selection valve in a one-to-one correspondence, the controller is used to control the sample loading valve interface 11 to communicate with one of the column interfaces or the detector interface, and under the control of the controller, the driving mechanism drives the valve core 2 of the column selection valve to rotate relative to the valve body 1, and when one of the column interfaces and another of the column interfaces are respectively connected to the two ends of the same chromatography column, the sample loading valve and the column selection valve and the chromatography column form a passage, thereby realizing the bypass, loading and flushing functions.
[0048] Specifically, in one embodiment of the present invention, the column selection valve is a nine-hole eight-channel valve, there are three chromatographic columns in the sample injection chromatography device, and one column selection valve includes six column interfaces, two detector interfaces and a loading valve interface 11. The three chromatographic columns are respectively the first chromatographic column, the second chromatographic column and the third chromatographic column, hereinafter referred to as column C1, column C2 and column C3; the two detector interfaces are respectively Out+ and Out-; the six column interfaces are respectively the first positive column interface, the first negative column interface, the second positive column interface, the second negative column interface, the third positive column interface and the third negative column interface, hereinafter referred to as C1+, C1-, C2+, C2-, C3+ and C3-; the first positive column interface, the second positive column interface and the third positive column interface correspond to the injection ends of the first chromatographic column, the second chromatographic column and the third chromatographic column, respectively, and the first negative column interface, the second negative column interface and the third negative column interface correspond to the sample outlet ends of the first chromatographic column, the second chromatographic column and the third chromatographic column, respectively.
[0049] like Figure 4As shown, the valve body 1 is disc-shaped, the loading valve interface 11 is arranged at the center of the valve body 1, Out+ and Out- are symmetrically arranged on both sides of the loading valve interface 11, and three column interfaces are symmetrically arranged between Out+ and Out-. The three column interfaces are evenly spaced between Out+ and Out-. From Out+ to Out-, they are C1+, C2+, and C2- respectively, and from Out- to Out+, they are C1-, C3-, and C3+ respectively. It should be noted that in this embodiment, two detector interfaces and six column interfaces, a total of eight interfaces, are evenly spaced and distributed on the inner side of the circumference of the valve body 1, and the distances from the eight interfaces to the loading valve interface 11 are equal.
[0050] like Figure 3 As shown, the upper surface of the valve core 2 is provided with four grooves, namely groove L1, groove L2, groove L3, and groove L4. The groove L1 is the main channel, which is connected from the sample loading valve interface 11 to one of the eight interfaces on the inner side of the circumference to realize bypass, sample loading, and flushing functions respectively:
[0051] (1) The mobile phase connected from the loading valve interface 11 is connected to the detector interface to realize the bypass function of the chromatography column, such as Figure 4-5 As shown;
[0052] (2) The mobile phase connected to the loading valve interface 11 is connected to the forward column interface to realize the loading function, such as Figure 6 , Figure 8 , Fig.10 As shown;
[0053] (3) The mobile phase connected from the loading valve interface 11 is connected to the reverse column interface to realize the column flushing function, such as Figure 7 , Fig. 9 , Fig.11 As shown;
[0054] The groove L2 connects two adjacent interfaces on the inner side of the circumference, the groove L3 connects two adjacent interfaces on the inner side of the circumference and is symmetrically distributed with respect to the groove L2, and the groove L4 connects two interfaces separated from each other on the inner side of the circumference. In one embodiment of the present invention, the connection method of the grooves L1, L2, L3, and L4 is as follows:
[0055] (1) The slot L1 connects the mobile phase received from the loading valve interface 11 to Out+ and Out- to realize the bypass function, or connects to C1+, C2+, and C3+ for loading, or connects to C1-, C2-, and C3- for column flushing;
[0056] (2) The slot L2 is connected to Out- and C1- to load the column C1, or is connected to Out+ and C1+ to wash the column C1;
[0057] (3) The slot L3 is connected to Out- and C2- to load the column C2, or is connected to Out+ and C3+ to wash the column C3;
[0058] (4) The slot L4 is connected to Out+ and C2+ to wash column C2, or is connected to Out- and C3- to load column C3.
[0059] It should be noted that the number, order and distribution positions of the above interfaces are only for illustration and are not intended to limit the protection scope of the present invention.
[0060] In one embodiment of the present invention, under the control of the controller, the driving mechanism drives the valve core 2 of the column selection valve to rotate relative to the valve body 1 to achieve the above-mentioned slot connection mode, so that the sample injection chromatography device has the following eight working positions:
[0061] (1) Figure 4 As shown, the sample injection chromatography device is in the first working position, and the mobile phase connected from the sample injection valve interface 11 flows directly to Out-, and flows to Out+ through a three-way pipe TEE, realizing the bypass 1 function;
[0062] (2) Figure 5 As shown, the sample injection chromatography device is in the second working position, and the mobile phase connected from the sample injection valve interface 11 flows directly to Out+, and flows to Out- through a three-way pipe TEE, realizing the bypass 2 function;
[0063] (3) Figure 6 As shown, the sample injection chromatography device is in the third working position, the mobile phase connected from the sample loading valve interface 11 is connected to C1+, connected to C1- through column C1, then connected to Out- from C1-, and then connected to the detector from Out-, and the sample loading status of column C1 is detected by the detector;
[0064] (4) Figure 7 As shown, the sample injection chromatography device is in the fourth working position, the mobile phase connected from the sample injection valve interface 11 is connected to C1-, connected to C1+ through column C1, then connected to Out+ from C1+, and then connected to the detector from Out+, and the flushing status of column C1 is detected by the detector;
[0065] (5) Figure 8As shown, the sample injection chromatography device is in the fifth working position, the mobile phase connected from the sample loading valve interface 11 is connected to C2+, connected to C2- through column C2, then connected to Out- from C2-, and then connected to the detector from Out-, and the sample loading status of column C2 is detected by the detector;
[0066] (6) Fig. 9 As shown, the sample injection chromatography device is in the sixth working position, the mobile phase connected from the sample loading valve interface 11 is connected to C2-, connected to C2+ through column C2, then connected to Out+ from C2+, and then connected to the detector from Out+, and the flushing status of column C2 is detected by the detector;
[0067] (7) Fig.10 As shown, the sample injection chromatography device is in the seventh working position, the mobile phase connected from the sample loading valve interface 11 is connected to C3+, connected to C3- through column C3, then connected to Out- from C3-, and then connected to the detector from Out-, and the sample loading status of column C3 is detected by the detector;
[0068] (8) Fig.11 As shown, the sample injection chromatography device is in the eighth working position, the mobile phase connected from the sample loading valve interface 11 is connected to C3-, connected to C3+ through column C3, then connected to Out+ from C3+, and then connected to the detector from Out+, and the flushing status of column C3 is detected by the detector;
[0069] It can be seen from the working position that when the bypass function is realized, the loading valve interface 11 is directly connected to the detector interface, and the mobile phase does not pass through any chromatography column.
[0070] In addition, in one embodiment of the present invention, the sample introduction chromatography device is further provided with a first pressure sensor and a second pressure sensor. The first pressure sensor is used to detect the system pressure to protect the chromatography column. The second pressure sensor is arranged behind the chromatography column, and by detecting the pressure difference loaded on the chromatography filler, an alarm threshold is pre-set to realize an overpressure alarm prompt, thereby protecting the filler from overpressure.
[0071] In one embodiment of the present invention, Figure 4-11 It can be seen that a test is provided which is usually used for a group of multiple sample sequences, and can also be used for a single type of multi-component sample test. Now take a complete case as an example. First, the system needs to be flushed. The valve is switched to Figure 4 state, and then perform column flushing respectively, and switch the valve to Figure 6 , Figure 8 , Fig.10 , respectively, to perform column forward flushing on column 1, column 2, and column 3, and to switch the valve to Figure 7, Fig. 9 , Fig.11 , respectively, to perform column reverse flushing on column 1, column 2, and column 3, and then switch the valve to Figure 6 , Figure 8 , Fig.10 , respectively, load the column 1, column 2, and column 3 with the sample in the forward direction, and detect it through the detector. If the previous column is full, it will automatically switch to the next column. When all columns are full, the valve will be switched to the next column through the software. Figure 7 , Fig. 9 , Fig.11 , perform reverse elution and collection on column 1, column 2, and column 3 respectively, detect the elution status through the detector, and repeat the test in this way.
[0072] In the above embodiment, the number of through slots is as follows: Figure 3 As shown, there are four (L1-L4). Obviously, the number of through slots is related to the number of chromatography columns of the sample injection chromatography device and the type of sample injection chromatography method. The present invention does not limit the number of through slots. For example, when the number of through slots is one, the sample injection chromatography device can also be implemented. Figure 6 Column 1 is flushed forward, Figure 7 Column 1 is backwashed, Figure 8 Column 2 is flushed forward, Fig.11 Column 3 is backwashed; if Fig.11 If the P connection C3- is changed to P connection C2-, one through slot can realize the forward and reverse flushing and bypass function of two chromatography columns; when the number of chromatography columns is three, to realize the forward and reverse flushing of three chromatography columns, the following settings can be made: Figure 3 The four through slots are shown; if more than four chromatography columns are to be flushed in the forward and reverse directions, more than four through slots need to be provided.
[0073] In one embodiment of the present invention, a method for controlling the injection of an injection chromatography device is provided, wherein the injection end of a target chromatography column is pre-connected to a target positive column interface, and the discharge end of the target chromatography column is pre-connected to a target negative column interface, and any one chromatography column in the controlled injection chromatography device is subjected to sample loading and / or backwashing. The specific steps of the control method are as follows:
[0074] For the loading control method, first, the loading valve interface 11 of the control column selection valve is connected to the target positive column interface, and then the valve core 2 of the control column selection valve is rotated until the target negative column interface is connected to the detector interface through the through groove on the valve core 2, and finally the loading valve is opened for loading.
[0075] For the reverse flushing control method, first, the loading valve interface 11 of the control column selection valve is connected to the target negative column interface, and then the valve core 2 is controlled to rotate until the target positive column interface is connected to the detector interface through the through groove 2 on the valve core, and finally the loading valve is opened for reverse flushing.
[0076] In addition, the column selection valve of the sample injection chromatography device includes a positive detector interface and a negative detector interface, and the control method also includes controlling the mobile phase bypass, and the specific control method is as follows:
[0077] Firstly, the positive detector interface and the negative detector interface are controlled to be connected to the detectors through a three-way joint. Secondly, the loading valve interface 11 of the column selection valve is controlled to be connected to the positive detector interface or the negative detector interface.
[0078] The concept of the present sample injection control method embodiment is the same as the working process of the sample injection chromatography device in the above-mentioned embodiment. The entire contents of the above-mentioned sample injection chromatography device embodiment are incorporated into the present sample injection control method embodiment by full reference and will not be repeated here.
[0079] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims
1. A sample injection chromatography device, characterized in that: Includes three chromatography columns and a column selection valve; The column selection valve comprises a valve body (1) and a disc-shaped valve core (2), wherein the valve core (2) is arranged on the valve body (1) and can rotate relative to the valve body (1) under the drive of a driving mechanism; The valve body (1) is provided with a loading valve interface (11) connected to an external loading valve, two detector interfaces connected to an external detector, and six column interfaces connected to an external chromatography column, and the loading valve interface (11) is controllably connected to one of the column interfaces; the loading valve interface (11) is arranged at the center of the valve body (1); two detector interfaces and six column interfaces, a total of eight interfaces, are evenly spaced and distributed on the inner side of the circumference of the valve body (1), and the distances from the eight interfaces to the loading valve interface (11) are equal, and the two detector interfaces are Out+ and Out-, respectively; The chromatography column comprises a first chromatography column, a second chromatography column and a third chromatography column, and the column interfaces comprise a first positive column interface, a first negative column interface, a second positive column interface, a second negative column interface, a third positive column interface and a third negative column interface, which are C1+, C1-, C2+, C2-, C3+ and C3- respectively; The first positive column interface, the second positive column interface, and the third positive column interface correspond to the injection ends of the first chromatography column, the second chromatography column, and the third chromatography column, respectively; the first negative column interface, the second negative column interface, and the third negative column interface correspond to the sample outlet ends of the first chromatography column, the second chromatography column, and the third chromatography column, respectively; Out+ and Out- are symmetrically arranged on both sides of the loading valve interface (11), and three column interfaces are symmetrically arranged between Out+ and Out-. The three column interfaces are equally spaced between Out+ and Out-. From Out+ to Out- in a counterclockwise direction, they are C1+, C2+, and C2-, and from Out- to Out+ in a counterclockwise direction, they are C1-, C3-, and C3+; The upper surface of the valve core (2) is provided with four grooves, namely groove L1 to groove L4, groove L1 is a main channel, connecting from the loading valve interface (11) to one of the eight interfaces on the inner side of the circumference; The groove L2 connects two adjacent interfaces on the inner side of the circumference, the groove L3 connects two adjacent interfaces on the inner side of the circumference and is symmetrically distributed with the groove L2, and the groove L4 connects two separated interfaces on the inner side of the circumference; The connection between slots L1 to L4 and the chromatography column and detector is as follows: Slot L1 connects the mobile phase received from the loading valve interface (11) to Out+ and Out- to realize the bypass function, or connects to C1+, C2+, C3+ for loading, or connects to C1-, C2-, C3- for column flushing; Slot L2 connects Out- and C1- to load column C1, or connects Out+ and C1+ to flush column C1; Slot L3 connects Out- and C2- to load column C2, or connects Out+ and C3+ to flush column C3; Slot L4 connects Out+ to C2+ to flush column C2, or connects Out- to C3- to load column C3; The sample injection chromatography device is also provided with a first pressure sensor and a second pressure sensor. The first pressure sensor is used to detect the system pressure. The second pressure sensor is arranged behind the chromatography column. By detecting the pressure difference loaded on the chromatography filler, an alarm threshold is pre-set to realize an overpressure alarm prompt.
2. The sample introduction chromatography device according to claim 1, characterized in that: It also includes a controller and a driving mechanism, wherein the controller is used to control the loading valve interface (11) of the column selection valve to communicate with one of the column interfaces or the detector interface; Under the control of the controller, the driving mechanism drives the valve core (2) of the column selection valve to rotate relative to the valve body (1).
3. A method for controlling the sample introduction of the sample introduction chromatography device according to claim 1, characterized in that: Control the loading and / or back flushing of any column in the sample injection chromatography device. Preliminarily connect the injection end of the target chromatography column to the interface of the target positive column, and connect the output end of the target chromatography column to the interface of the target negative column; The sample loading control method comprises: controlling the sample loading valve interface of the column selection valve to be connected with the target positive column interface, controlling the valve core of the column selection valve to rotate until the target negative column interface is connected with the detector interface through the through groove on the valve core; and then opening the sample loading valve to load the sample; The backwash control method includes: controlling the loading valve interface of the column selection valve to communicate with the target negative column interface, controlling the valve core to rotate until the target positive column interface and the detector interface are connected through the through groove on the valve core; and then opening the loading valve for backwashing.
4. The injection control method according to claim 3, wherein the column selection valve of the injection chromatography device comprises a positive detector interface and a negative detector interface, wherein: The control method further includes controlling the mobile phase bypass, including: The positive detector interface and the negative detector interface are controlled to be connected to the detector through a three-way joint; and the loading valve interface of the column selection valve is controlled to be connected to the positive detector interface or the negative detector interface.
Citation Information
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