A multi-channel liquid exchange device for chromatography-mass spectrometry

By introducing a multi-channel liquid exchange device into the chromatographic mass spectrometer, using a negative pressure pump and a stepped channel design, the problem of residual liquid contamination during the switching process is solved, and efficient and accurate detection results and equipment life are achieved.

CN120254151BActive Publication Date: 2025-08-26RELAIS (HANGZHOU) MEDICAL TECH CO LTD
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Patent Information

Application Number
CN202510712603.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-05-30
Publication Date
2025-08-26
Estimated Expiration
2045-05-30

AI Technical Summary

Technical Problem

The switching mechanism of the existing chromatographic mass spectrometer is prone to residual liquid during rotation, resulting in contamination, affecting the accuracy of the detection result, and the utilization rate of the mass spectrometer is low.

Method used

A multi-channel liquid exchange device is adopted, including a transfer box, cover plate, bottom plate, cleaning pipe, negative pressure pump, etc. Through negative pressure suction and step-shaped channel design, the dripping of liquid on the hanging wall is reduced, the detection accuracy is improved, and the pipeline layout is optimized.

Benefits of technology

It effectively reduces the risk of pollution during the switching process, improves the accuracy of detection results and the utilization rate of the mass spectrometer, and extends the equipment life.

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Abstract

The present application relates to a multi-channel liquid exchange device for a chromatography-mass spectrometry instrument, and relates to the technical field of chromatography-mass spectrometry instruments. The device achieves the following effects through the coordinated efforts of components such as transfer channels, cleaning tubes, isolation plates, and negative pressure pumps: Highly efficient pollution prevention: In the non-liquid supply state, residual liquid and air are sucked out by a negative pressure pump, which significantly reduces dripping of liquid hanging on the wall and avoids contamination of the switching surface; Precise channel switching: The transfer channels distributed in a stepped array optimize the liquid flow path, and the precise engagement of the drive gear and the rack ensures that the switching process is fast and the positioning is accurate; Flexible cleaning and maintenance: The design of the series channels combined with the turbulent vanes and vibration springs can flush the channels centrally or individually, greatly improving the cleaning efficiency. At the same time, the filter bags and staggered bars effectively intercept droplets to prevent secondary contamination; Extended equipment life: The design of the transfer rack and the flexible connecting pipe reduces pipe bending and mechanical wear, reduces maintenance requirements, and improves the long-term stability of the system.
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Description

Technical Field

[0001] The present application relates to the technical field of chromatography-mass spectrometry, and in particular to a multi-channel liquid exchange device for a chromatography-mass spectrometry instrument. Background Art

[0002] A mass spectrometer is an instrument used to separate and detect different isotopes. Based on the principle that charged particles can be deflected in an electromagnetic field, a mass spectrometer detects substances based on the mass differences of their atoms, molecules, or molecular fragments. This allows for effective analysis of a substance's constituent elements and composition. However, in practice, the substances being measured are often complex mixtures, making the mass spectra obtained by a mass spectrometer complex and difficult to analyze. Therefore, a chromatograph is often combined with a mass spectrometer to separate and analyze the mixture through liquid chromatography or gas chromatography. The separated substances are then introduced into a mass spectrometer for mass spectrometry analysis.

[0003] The Chinese patent with the existing authorization announcement number CN117571897B discloses a liquid chromatography-mass spectrometry instrument and a switching device, which includes a waste liquid barrel and a switching mechanism. The waste liquid barrel is fixedly connected to a waste liquid pipe. The switching mechanism includes a frame, a valve core, an upper valve body, a lower valve body, a chassis and a switching member that drives the valve core and the chassis to rotate. The upper valve body is fixedly connected to the frame, the lower valve body is rotatably connected to the frame, and the upper valve body is provided with a plurality of feed cavities. The feed cavities are arranged along the periphery of the upper valve body. The valve body is arranged at an angle to the center of the valve core. The lower valve body is provided with a discharge cavity and a waste liquid cavity. The valve core is provided with a plurality of liquid inlets, liquid outlets and waste liquid outlets. The liquid inlets are arranged at equal angles and intervals along the upper end of the valve core. The liquid outlets and waste liquid outlets are symmetrically arranged at the lower end of the valve core about the vertical axis of the valve core. A pipeline is connected between one of the liquid inlets and the liquid outlet, and the waste liquid outlet is connected to a waste liquid pipeline. The remaining liquid inlets are all connected to the waste liquid pipeline. The lower valve body is fixedly connected to the chassis, and the waste liquid pipe is fixedly connected to the chassis. When analyzing the same sample, the liquid chromatograph generally takes a long time to separate and analyze the sample. When the chromatograph and the mass spectrometer are connected in parallel one-to-one, the actual analysis time of the mass spectrometer is short. It is often in an idle state and the mass spectrometer keeps working continuously, which makes the utilization rate of the mass spectrometer low. Therefore, the technical solution adopted in the related art is to combine multiple chromatographs with a mass spectrometer, and use a switching mechanism to switch the pipelines to selectively connect the liquid outlet pipes of multiple chromatographs with the liquid inlet pipe of the mass spectrometer.

[0004] The above-mentioned related technologies have the following defects: the general principle of the switching mechanism is to connect the liquid outlet pipe of the chromatograph and the liquid inlet pipe of the mass spectrometer to the switching mechanism, and a relatively rotatable switching surface is provided inside the switching mechanism. When the channels of the two switching surfaces are connected, normal liquid supply is achieved. When the channels of the two switching surfaces are disconnected, the switching surface can be used to block the corresponding channels, thereby achieving the opening and closing control between different pipelines. However, during the actual switching process, some liquid hanging on the wall is likely to remain at the end of the channel near the switching surface. Therefore, the switching mechanism is likely to apply the residual liquid to the switching surface during rotation, which is likely to cause contamination and may affect the accuracy of the final detection results. Therefore, it needs to be improved. Summary of the Invention

[0005] In order to reduce the impact of residual wall liquid in the pipeline on the switching surface during rotation, the present application provides a multi-channel liquid exchange device for a chromatography-mass spectrometry instrument.

[0006] The multi-channel liquid exchange device of the chromatography-mass spectrometry instrument provided in this application adopts the following technical solution:

[0007] A multi-channel liquid exchange device for a chromatograph-mass spectrometer, comprising a chromatograph liquid outlet pipe connected to the chromatograph, a mass spectrometer liquid inlet pipe connected to the mass spectrometer, and a switching mechanism connected between the chromatograph liquid outlet pipe and the mass spectrometer liquid inlet pipe. The switching mechanism comprises a transfer box, a cover plate rotatably connected to the top of the transfer box, and a base plate rotatably connected to the bottom of the transfer box. The chromatograph liquid outlet pipe is connected to the cover plate, and the mass spectrometer liquid inlet pipe is connected to the base plate. The transfer box has a transfer channel extending therethrough, and the transfer channel is connected to the corresponding chromatograph liquid outlet pipe and mass spectrometer liquid inlet pipe.

[0008] A cleaning tube is provided inside the chromatographic liquid outlet pipe, and the bottom of the cleaning tube is connected to an isolation plate for blocking the bottom of the chromatographic liquid outlet pipe via a flexible connecting tube. A cleaning channel is provided inside the isolation plate, and the flexible connecting tube is connected to the cleaning channel, and the cleaning channel is arranged at an end away from the flexible connecting tube toward the chromatographic liquid outlet pipe. The top of the cleaning tube extends out of the chromatographic liquid outlet pipe and is connected to an air supply pipe and a liquid supply pipe via a conversion valve.

[0009] A negative pressure pump is provided on the side of the chromatographic liquid outlet pipe.

[0010] By adopting this technical solution, efficient switching between the chromatograph outlet and the mass spectrometer inlet is achieved, effectively reducing contamination of the equipment by liquid deposited on the wall during the switching process. Specifically, the switching mechanism, consisting of a transfer box, cover plate, and base plate, combined with the design of a cleaning tube, isolation plate, and negative pressure pump, ensures normal liquid circulation in the liquid supply state, while reducing dripping of liquid deposited on the wall through negative pressure suction in the non-liquid supply state, thereby improving the accuracy of test results and extending the service life of the equipment.

[0011] The specific switching process is as follows:

[0012] In the liquid supply state, the chromatographic liquid outlet pipe is coaxially placed with the corresponding transfer channel, and the conversion valve and negative pressure pump are in the closed state. In this state, the isolation plate swings downward under its own gravity and enters the transfer channel. At this time, the bottom of the chromatographic liquid outlet pipe is in the open state, and liquid can be supplied normally.

[0013] In the non-liquid supply state, the chromatographic liquid outlet pipe and the corresponding transfer channel rotate relative to each other. During this process, the conversion valve is adjusted to a state where the air supply pipe and the cleaning pipe are connected, and the negative pressure pump is turned on. When the top wall of the transfer box finally pushes the isolation plate upward until the isolation plate blocks the bottom of the chromatographic liquid outlet pipe, the negative pressure pump maintains the negative pressure state inside the chromatographic liquid outlet pipe, and sucks the air inside the transfer channel and the air inside the cleaning channel and the cleaning pipe from bottom to top, thereby reducing the dripping of the wall liquid in the chromatographic liquid outlet pipe;

[0014] Before switching to connect another chromatographic liquid outlet tube to the corresponding transfer channel, close the conversion valve and the negative pressure pump. When the other chromatographic liquid outlet tube rotates to be coaxial with the corresponding transfer channel, liquid supply to the other chromatographic liquid outlet tube can be achieved.

[0015] Preferably, several of the transfer channels are arranged in a stepped manner and each has a liquid inlet end, a middle section and a liquid outlet end that are connected in sequence, the liquid inlet end extends to the top wall of the transfer box, and the liquid outlet end extends to the bottom wall of the transfer box. The middle sections of several of the transfer channels are arranged in sequence along the thickness direction of the transfer box and the projection position relationship is arranged in an array with the center of the transfer box as the center of the circle.

[0016] By adopting this technical solution, the transfer channels are arranged in a stepped pattern, divided into an inlet, an intermediate section, and an outlet. This allows for orderly arrangement of the channels within a limited space, improving space utilization while facilitating pipe connections. The design of extending the inlet to the top wall of the transfer box and the outlet to the bottom wall ensures a smooth liquid flow path and reduces the possibility of liquid residue. The intermediate sections are arranged sequentially along the thickness of the transfer box, with their projected positions arranged in an array centered around the center of the transfer box. This further optimizes the channel layout, improves switching accuracy, and reduces the risk of cross-contamination.

[0017] Preferably, several of the transfer channels are connected in series via a series channel, and the series channel is provided with a series valve.

[0018] By adopting the above technical solution, when several transfer channels need to be flushed centrally, the series valves can be opened to connect the several transfer channels in an S-shaped series, so that the several transfer channels can be flushed centrally after being used once, achieving a more energy-saving effect.

[0019] Preferably, a turbulent vane is provided inside the series channel, and the turbulent vane is spiral and arranged parallel to the axial direction of the series channel.

[0020] By adopting the above technical solution, the provision of turbulent vanes can effectively enhance the turbulence of the liquid within the series channels. Specifically, when the liquid flows through the series channels, the spiral turbulent vanes guide the liquid into a rotating flow, thereby increasing the contact area between the liquid and the channel walls and helping to remove residual matter within the channel. This structural design also promotes more uniform mixing of the liquid, further improving flushing efficiency and ensuring the cleanliness of the transfer channel during the centralized flushing process.

[0021] Preferably, the turbulent vanes are connected to the series channels via a vibration spring.

[0022] By adopting this technical solution, the turbulent vanes and the series channel are connected by a vibration spring, which generates vibrations during the liquid flushing process, enhancing the liquid's turbulence and further improving cleaning efficiency, ensuring that residual matter in the transfer channel is completely removed. Furthermore, the vibration spring design effectively prevents damage to the equipment caused by impact forces during the flushing process, thereby extending the device's service life.

[0023] Preferably, a transfer rack is fixedly arranged between the cover plate and the bottom plate.

[0024] By adopting this technical solution, the transfer rack simplifies the channel switching process. Subsequent channel switching requires only rotating the transfer box, eliminating the need to rotate the cover and base plates separately. This prevents the chromatograph and mass spectrometer outlet tubes, which are connected to the cover and base plates, from bending due to frequent switching, significantly extending the life of the tubes.

[0025] Preferably, the transfer rack is rotatably provided with a driving gear, the side wall of the transfer box is provided with a driving rack, the driving gear is meshed with the driving rack, and the transfer rack is further provided with a transfer driving member for driving the driving gear to rotate.

[0026] By implementing this technical solution, precise rotational control of the transfer box is achieved. Specifically, the coordination of the drive gear and drive rack ensures stability and accuracy during the transfer box's rotation, thereby improving operational reliability when switching between different chromatographic outlet tubes and the transfer channel. Furthermore, the design of the transfer drive further simplifies the operational process, enhances the automation level of the equipment, reduces errors caused by human intervention, and ensures good sealing and rapid switching between channels during liquid exchange.

[0027] Preferably, the cover plate is connected to a flushing pipe, and the bottom plate is connected to a recovery pipe.

[0028] By adopting this technical solution, when a transfer channel needs to be flushed, the transfer box is rotated to connect the corresponding transfer channel to the flushing pipe and recovery pipe, thus flushing the specific transfer channel. The waste liquid can then be collected through the recovery pipe. This design effectively removes residual materials in the transfer channel, preventing cross-contamination, while ensuring that the waste liquid is properly handled, improving the cleaning efficiency and environmental performance of the entire system.

[0029] Preferably, the negative pressure pump is connected to a filter bag, the bottom of the filter bag is open, and a plurality of bars are provided inside the filter bag, and the plurality of bars are staggered.

[0030] By employing this technical solution, the internal ribs of the filter bag effectively absorb stray droplets from the airflow. Specifically, the staggered ribs restrict the gas flow path, forcing the airflow containing droplets to change direction multiple times as it passes through the ribs, increasing the chances of droplets colliding with the ribs. This structure not only prevents droplets from being discharged with the airflow and causing secondary contamination to the external environment, but also improves the cleaning efficiency and stability of the negative pressure system. The open bottom design of the filter bag facilitates regular cleaning of absorbed liquid, ensuring long-term stable operation of the system.

[0031] A liquid exchange method for a multi-channel liquid exchange device based on a chromatogram-mass spectrometer. In the liquid supply state, the chromatogram outlet pipe is coaxially placed with the corresponding transfer channel, and the conversion valve and negative pressure pump are closed. In this state, the isolation plate swings downward under its own gravity and enters the transfer channel. At this time, the bottom of the chromatogram outlet pipe is in the open state, and normal liquid supply can be achieved.

[0032] In the non-liquid supply state, the chromatographic liquid outlet pipe and the corresponding transfer channel rotate relative to each other. During this process, the conversion valve is adjusted to a state where the air supply pipe and the cleaning pipe are connected, and the negative pressure pump is turned on. When the top wall of the transfer box finally pushes the isolation plate upward until the isolation plate blocks the bottom of the chromatographic liquid outlet pipe, the negative pressure pump maintains the negative pressure state inside the chromatographic liquid outlet pipe, and sucks the air inside the transfer channel and the air inside the cleaning channel and the cleaning pipe from bottom to top, thereby reducing the dripping of the wall liquid in the chromatographic liquid outlet pipe;

[0033] Before switching to connect another chromatographic liquid outlet tube to the corresponding transfer channel, close the conversion valve and the negative pressure pump. When the other chromatographic liquid outlet tube rotates to be coaxial with the corresponding transfer channel, liquid supply to the other chromatographic liquid outlet tube can be achieved.

[0034] By adopting the above technical solution, it is possible to ensure that the chromatographic liquid outlet tube and the transfer channel are accurately docked and normally supply liquid in the liquid supply state, while effectively reducing the dripping of liquid hanging on the wall of the chromatographic liquid outlet tube in the non-liquid supply state, improving the cleanliness and reliability of the switching process, thereby improving the accuracy of the overall detection results. Specifically:

[0035] In the liquid supply state, the isolation plate swings downward into the transfer channel by its own gravity, ensuring that the bottom of the chromatographic liquid outlet tube is open to achieve smooth liquid supply.

[0036] In the non-liquid supply state, the conversion valve is adjusted to connect the air supply pipe and the cleaning pipe, and the negative pressure inside the chromatographic liquid outlet pipe is maintained with the help of a negative pressure pump to suck out the air in the transfer channel, cleaning channel and cleaning pipe, significantly reducing the risk of liquid dripping from the wall.

[0037] During the switching process, the conversion valve and the negative pressure pump are closed and the liquid supply operation is resumed after the other chromatographic liquid outlet tube is rotated into place, realizing efficient and stable multi-channel liquid exchange function.

[0038] In summary, this application includes at least one of the following beneficial technical effects:

[0039] 1. In the non-liquid supply state, the air inside the chromatographic liquid outlet pipe and the air in the cleaning channel are extracted by a negative pressure pump, effectively reducing the dripping of liquid on the wall, significantly reducing the contamination of the switching surface by residual liquid during the switching process, and improving the accuracy of the test results;

[0040] 2. The transfer channels are arranged in a stepped and array-like manner, which optimizes the pipeline layout, facilitates the simultaneous management and rapid switching of multiple channels, and improves overall work efficiency;

[0041] 3. Flushing pipes and recovery pipes are set up to flush specific transfer channels separately when needed and collect waste liquid in a centralized manner to avoid secondary pollution, thereby enhancing the cleanliness and maintenance convenience of the system. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] Figure 1 This is a schematic structural diagram of an embodiment of the present application;

[0043] Figure 2 This is a structural diagram illustrating the connection relationship between the transfer box and the transfer drive member in an embodiment of the present application;

[0044] Figure 3 This is a structural diagram illustrating the connection relationship between the transfer channel, the mass spectrometer liquid inlet pipe, and the chromatographic liquid outlet pipe in the embodiment of the present application;

[0045] Figure 4 This is a structural diagram for illustrating the positional relationship between the transfer channel and the series channel in an embodiment of the present application;

[0046] Figure 5 This is a structural diagram for illustrating the connection relationship of series channels in an embodiment of the present application;

[0047] Figure 6 This is a structural diagram illustrating the connection relationship between the turbulent vanes and the series channels in an embodiment of the present application;

[0048] Figure 7 This is a schematic diagram of the structure in the embodiment of the present application, showing that the isolation plate is flipped downward so that the bottom of the chromatographic liquid outlet tube is open;

[0049] Figure 8 This is a schematic diagram of the structure in the embodiment of the present application, showing that the isolation plate is flipped upward to close the bottom of the chromatographic liquid outlet pipe;

[0050] Figure 9 This is a structural diagram used to illustrate the connection relationship between the cleaning pipe, the connecting pipe and the isolation plate in the embodiment of the present application.

[0051] In the picture:

[0052] 1. Transfer box; 10. Transfer channel; 11. Cover plate; 12. Bottom plate; 13. Transfer rack; 14. Drive gear; 15. Drive rack; 16. Transfer drive element; 17. Flushing pipe; 18. Recovery pipe;

[0053] 2. Chromatograph; 21. Chromatograph outlet pipe; 22. Cleaning pipe; 23. Connecting pipe; 24. Isolation plate; 240. Cleaning channel; 25. Switching valve; 26. Air supply pipe; 27. Liquid supply pipe; 28. Negative pressure pump; 29. ​​Filter bag; 291. Stop bar;

[0054] 3. Mass spectrometer; 31. Mass spectrometer liquid inlet pipe;

[0055] 4. Series channel; 41. Series valve; 42. Turbine vane; 43. Vibration spring. DETAILED DESCRIPTION

[0056] The following will be combined with the accompanying drawings to clearly and completely describe the technical solutions in the embodiments of the present invention. The described embodiments are only possible technical implementations of the present invention and are not all possible implementations. Those skilled in the art can fully combine the embodiments of the present invention to derive other embodiments without creative work, and these embodiments are also within the scope of protection of the present invention.

[0057] The inventors of the present application have discovered that mass spectrometers, as a type of precision analytical equipment, are widely used in the fields of chemistry, biology, medicine, etc. However, traditional switching devices are prone to cross-contamination due to residual liquid in the pipeline during the switching process, which seriously affects the reliability of the detection data. For example, although the rotating disk design can achieve multi-channel switching, its mechanical contact surface is prone to carry residual liquid to the adjacent channel during rotation, resulting in sample contamination. To this end, the present application mainly adopts a multi-channel liquid exchange device for a chromatography-mass spectrometry instrument, including a transfer box, a cover plate, a bottom plate, a chromatography outlet pipe, a mass spectrometry inlet pipe and other components and related cleaning components, which achieves the effect of reducing residual liquid contamination and improving detection accuracy. The following is a further detailed description of the present application. Example

[0058] Reference Figure 1 and Figure 2 The multi-channel liquid exchange device of the chromatography-mass spectrometer provided in the embodiment of the present application includes a transfer box 1, a cover plate 11 rotatably connected to the top of the transfer box 1, and a base plate 12 rotatably connected to the bottom of the transfer box 1. The transfer box 1, the cover plate 11 and the base plate 12 are connected by bearings, which ensures the rotation flexibility while reducing wear. Specifically, a transfer rack 13 in the form of a frame is fixedly arranged between the cover plate 11 and the base plate 12. A drive gear 14 is arranged on the side of the transfer rack 13. A section of a drive rack 15 made of metal is welded to the side wall of the transfer box 1. The drive gear 14 is tightly engaged with the drive rack 15. The transfer rack 13 is also provided with a stepping motor as a transfer drive member 16 for driving the drive gear 14 to rotate. By controlling the stepping motor, the transfer box 1 can be driven to rotate precisely relative to the cover plate 11 and the base plate 12, so as to automatically and quickly complete the selection and switching process of the required channels.

[0059] Reference Figure 1 and Figure 2 The cover plate 11 is connected to a number of chromatographic liquid outlet pipes 21 and a flushing pipe 17. The top of the chromatographic liquid outlet pipe 21 is connected to the chromatograph 2 to receive the liquid processed by the chromatograph 2, and the top of the flushing pipe 17 is connected to the cleaning liquid. The bottom plate 12 is connected to a number of mass spectrometer liquid inlet pipes 31 and a recovery pipe 18. The mass spectrometer liquid inlet pipe 31 is used to transport the liquid processed by the chromatograph 2 to the mass spectrometer 3 for analysis, and the recovery pipe 18 is used to collect the waste liquid after flushing. The specific connection method between the multiple pipe ends and the cover plate 11 or the bottom plate 12 can be installed using a quick-release connector to facilitate later maintenance.

[0060] Reference Figure 3 and Figure 4 The transfer box 1 has a plurality of transfer channels 10 extending therethrough. When the transfer box 1 is rotated to a specific angle, the two ends of the transfer channel 10 are respectively connected to the corresponding chromatographic liquid outlet pipe 21 and the mass spectrometer liquid inlet pipe 31, or the two ends of the transfer channel 10 are respectively connected to the flushing pipe 17 and the recovery pipe 18, or the two ends of the transfer channel 10 are respectively closed by the cover plate 11 and the bottom plate 12.

[0061] The plurality of transfer channels 10 are arranged in a stepped manner and in a Z-shaped distribution with two turning points. Therefore, the plurality of transfer channels 10 form a liquid inlet end, a middle section and a liquid outlet end that are connected in sequence. The liquid inlet end extends to the top wall of the transfer box 1 and is sealed and docked with a conical sealing ring. The liquid outlet end extends to the bottom wall of the transfer box 1 and is also installed and sealed with a conical sealing ring of the same specification. The middle sections of the plurality of transfer channels 10 are arranged in sequence along the thickness direction of the transfer box 1 and the projected position relationship is distributed in an array with the center of the transfer box 1 as the center of the circle. In addition, the plurality of transfer channels 10 are arranged in series through a series channel 4, and an electrically controlled series valve 41 is installed on the series channel 4. When a plurality of transfer channels 10 need to be flushed collectively, an S-shaped water flow path can be established by opening all the series valves 41 to achieve efficient flushing.

[0062] Reference Figure 5 and Figure 6 The series channel 4 is internally provided with a flow-turbulating vane 42. The flow-turbulating vane 42 is spiral-shaped and arranged axially parallel to the series channel 4. The flow-turbulating vane 42 is connected to the series channel 4 by a vibration spring 43 made of high-strength stainless steel to ensure stable operation under long-term vibration conditions. This structure significantly enhances the flushing force and thoroughly cleans the residual liquid. In this embodiment, each section of the transfer channel 10 is provided with two series valves 41, and the two series valves 41 are respectively located on both sides of the flow-turbulating vane 42. Under normal conditions, both ends of the series channel 4 are adjusted to a closed state by the series valve 41 to prevent the series channel 4 from being connected to the interior of the transfer channel 10 under normal liquid supply conditions, causing sample contamination.

[0063] Reference Figure 7 、 Figure 8 and Figure 9 The chromatographic liquid outlet pipe 21 is connected to a cleaning pipe 22 from the side wall. A portion of the cleaning pipe 22 extends into the interior of the chromatographic liquid outlet pipe 21, and the bottom of the cleaning pipe 22 extends to the bottom of the chromatographic liquid outlet pipe 21. The bottom of the cleaning pipe 22 is connected to an isolation plate 24 through a flexible silicone connecting pipe 23. The isolation plate 24 itself is also made of an elastic material. When the chromatographic liquid outlet pipe 21 is connected to the transfer channel 10, the isolation plate 24 can naturally fall down and extend into the interior of the transfer channel 10. At this time, the chromatographic liquid outlet pipe 21 and the transfer channel 10 are in a connected state. When rotation occurs and the chromatographic liquid outlet pipe 21 and the transfer channel 10 gradually deviate, the abutment surface will push the isolation plate 24 to flip upward until it returns to the interior of the chromatographic liquid outlet pipe 21 and blocks the bottom of the chromatographic liquid outlet pipe 21.

[0064] A cleaning channel 240 is also provided within the isolation plate 24. The flexible connecting tube 23 is connected to the cleaning channel 240, with the end of the cleaning channel 240, distal from the flexible connecting tube 23, being positioned toward the chromatogram outlet tube 21. The top of the cleaning tube 22 extends from the side wall of the chromatogram outlet tube 21 and is connected to an air supply tube 26 and a liquid supply tube 27 via a conversion valve 25 secured by a threaded joint. The conversion valve 25 is a three-way valve, and adjustment of the conversion valve 25 allows for selection between air supply and liquid supply. Furthermore, a vacuum-type negative pressure pump 28 is provided on the side of the chromatogram outlet tube 21. This negative pressure pump 28 maintains a negative pressure within the chromatogram outlet tube 21 when the chromatogram outlet tube 21 is not supplying liquid. In conjunction with the air supply tube 26, the air at the bottom of the chromatogram outlet tube 21 is pumped upward to the negative pressure pump 28 and discharged from the chromatogram outlet tube 21. This process effectively removes liquid adhering to the wall and reduces secondary contamination caused by dripping liquid. When the bottom of the chromatographic liquid outlet pipe 21 is closed, the negative pressure pump 28 can be turned off to adjust the switching valve 25 to the liquid supply state. In this state, the liquid supply pipe 27 can be used to clean the inside of the chromatographic liquid outlet pipe 21.

[0065] Furthermore, the outlet of the negative pressure pump 28 is connected to a filter bag 29. The bottom opening of the filter bag 29 facilitates exhaust. Inside the bag, multiple layers of staggered bars 291 are arranged. These bars are made of a fiber material with a high water absorption capacity. Liquid-containing gas entering the filter bag 29 is forced to change direction and strike the surface of the bars 291 multiple times, ultimately effectively intercepting and capturing most of the tiny droplets, preventing secondary contamination of the surrounding air.

[0066] The implementation principle of this embodiment is:

[0067] By introducing a cleaning assembly consisting of a cleaning tube 22, a flexible connecting tube 23, and an isolation plate 24, effective cleaning of the inside of the chromatographic liquid outlet tube 21 is achieved, reducing the risk of contamination of the switching surface by the hanging liquid. Especially in the non-liquid supply state, a stable negative pressure environment is formed with the help of the negative pressure pump 28, which further improves the cleaning effect. Compared with the traditional single reliance on mechanical closure, this design scheme takes into account functionality and reliability, and greatly improves the operational stability of the equipment. The newly added transfer rack 13 and its drive system optimize the overall architecture, which not only simplifies the switching process but also improves the degree of automation. Various auxiliary facilities such as the series channel 4, the turbulent rotor 42, the vibration spring 43 and the filter bag 29 work together to fully guarantee the cleanliness level of the system and ensure that each switch can achieve the best performance.

[0068] The beneficial effects of this embodiment are further reflected in:

[0069] The stepped layout of the transfer channel 10: by arranging the middle sections of the transfer channel 10 in sequence along the thickness direction of the transfer box 1 and distributing them in an array around the center, the space utilization is optimized.

[0070] The flexible connecting tube 23 and the isolation plate 24 work together: The flexible silicone connecting tube 23 is both corrosion-resistant and elastic, and its angle can be adaptively adjusted under the weight of the isolation plate 24 to ensure a tight seal. The guiding design of the cleaning channel 240 within the isolation plate 24 directs the airflow to flush the wall of the chromatographic outlet tube 21, further reducing the adhesion of residual liquid.

[0071] Enhanced cleaning by the turbulent vanes 42 and the vibration springs 43: The spiral turbulent vanes 42 generate eddies when the liquid flows through. Combined with the high-frequency vibration of the vibration springs 43, the turbulent intensity of the liquid is enhanced, effectively stripping away deposits on the channel wall. This design is particularly suitable for cleaning scenarios with high-viscosity liquids.

[0072] The droplet interception effect of the filter bag 29 and the baffle 291: the multi-layer staggered baffles 291 in the filter bag 29 force the liquid-containing airflow to turn multiple times, which increases the droplet collision interception rate. The bottom opening design facilitates regular cleaning or drying to prevent the filter bag 29 from being too wet, ensuring the long-term stable operation of the negative pressure system.

[0073] This application achieves the following core advantages through the comprehensive application of the above technical solutions:

[0074] Cross-contamination control: The combination of negative pressure suction and directional cleaning technology reduces the risk of residual liquid contamination during the switching process, ensuring the purity and accuracy of the test data;

[0075] Convenient operation: The introduction of the transfer rack 13 and the automated drive system simplifies the channel switching process, making it particularly suitable for high-throughput detection scenarios.

[0076] Energy saving and environmental protection: The centralized flushing mode of the series channel 4 saves the amount of cleaning fluid compared to the traditional channel-by-channel cleaning. Combined with the design of the waste liquid recovery pipe 18, it further reduces resource waste and environmental burden.

[0077] Improved durability: The low-wear design of the transfer box 1 and pipelines extends the life of key components such as pipelines, significantly reducing the equipment's life cycle cost.

[0078] The present application also discloses a multi-channel liquid exchange method for a chromatography-mass spectrometer. The method is based on a multi-channel liquid exchange device for a chromatography-mass spectrometer. In the liquid supply state, the chromatographic liquid outlet pipe 21 is coaxially placed with the corresponding transfer channel 10, and the conversion valve 25 and the negative pressure pump 28 are in the closed state. In this state, the isolation plate 24 swings downward under its own gravity and enters the interior of the transfer channel 10. At this time, the bottom of the chromatographic liquid outlet pipe 21 is in the open state, and normal liquid supply can be achieved.

[0079] In the non-liquid supply state, the chromatographic liquid outlet pipe 21 and the corresponding transfer channel 10 rotate relative to each other. During this process, the switching valve 25 is adjusted to a state where the air supply pipe 26 is connected to the cleaning pipe 22, and the negative pressure pump 28 is turned on. When the top wall of the transfer box 1 finally pushes the isolation plate 24 upward until the isolation plate 24 blocks the bottom of the chromatographic liquid outlet pipe 21, the negative pressure pump 28 maintains the negative pressure state inside the chromatographic liquid outlet pipe 21, and sucks the air inside the transfer channel 10 and the air inside the cleaning channel 240 and the cleaning pipe 22 from bottom to top, thereby reducing the dripping of the wall liquid in the chromatographic liquid outlet pipe 21;

[0080] Before switching to connect another chromatographic liquid outlet pipe 21 with the corresponding transfer channel 10, close the conversion valve 25 and the negative pressure pump 28. When the other chromatographic liquid outlet pipe 21 rotates to be coaxial with the corresponding transfer channel 10, the liquid supply of the other chromatographic liquid outlet pipe 21 can be realized.

[0081] By adopting the above technical solution, it is possible to ensure that the chromatographic liquid outlet tube 21 is accurately docked with the transfer channel 10 and supplies liquid normally in the liquid supply state. At the same time, in the non-liquid supply state, the dripping of the liquid hanging on the wall in the chromatographic liquid outlet tube 21 is effectively reduced, thereby improving the cleanliness and reliability during the switching process, thereby improving the accuracy of the overall detection results.

[0082] Specifically:

[0083] In the liquid supply state, the isolation plate 24 swings downward into the interior of the transfer channel 10 by its own gravity, ensuring that the bottom of the chromatographic liquid outlet pipe 21 is open to achieve smooth liquid supply.

[0084] In the non-liquid supply state, the conversion valve 25 is adjusted to connect the air supply pipe 26 with the cleaning pipe 22, and the negative pressure state inside the chromatographic liquid outlet pipe 21 is maintained with the help of the negative pressure pump 28, so that the air in the transfer channel 10, the cleaning channel 240 and the cleaning pipe 22 is sucked out, which significantly reduces the risk of liquid dripping on the wall.

[0085] During the switching process, the conversion valve 25 and the negative pressure pump 28 are closed and the liquid supply operation is resumed after the other chromatographic liquid outlet pipe 21 is rotated into place, thereby achieving an efficient and stable multi-channel liquid exchange function.

[0086] The above are all preferred embodiments of the present application, and are not intended to limit the scope of protection of the present application. Therefore, any equivalent changes made based on the structure, shape, and principle of the present application should be included in the scope of protection of the present application.

Claims

1. A multi-channel liquid exchange device for a chromatograph-mass spectrometer, comprising a chromatograph liquid outlet pipe (21) connected to a chromatograph (2), a mass spectrometer liquid inlet pipe (31) connected to a mass spectrometer (3), and a switching mechanism connected between the chromatograph liquid outlet pipe (21) and the mass spectrometer liquid inlet pipe (31), characterized in that: The switching mechanism comprises a transfer box (1), a cover plate (11) rotatably connected to the top of the transfer box (1), and a bottom plate (12) rotatably connected to the bottom of the transfer box (1); the chromatographic liquid outlet pipe (21) is connected to the cover plate (11); the mass spectrometer liquid inlet pipe (31) is connected to the bottom plate (12); the transfer box (1) has a transfer channel (10) arranged therethrough; the transfer channel (10) is connected to the corresponding chromatographic liquid outlet pipe (21) and the mass spectrometer liquid inlet pipe (31); A cleaning tube (22) is provided inside the chromatographic liquid outlet pipe (21), and the bottom of the cleaning tube (22) is connected to an isolation plate (24) for blocking the bottom of the chromatographic liquid outlet pipe (21) through a flexible connecting tube (23). A cleaning channel (240) is provided inside the isolation plate (24), and the flexible connecting tube (23) is connected to the cleaning channel (240), and the cleaning channel (240) is provided at one end away from the flexible connecting tube (23) toward the chromatographic liquid outlet pipe (21). The top of the cleaning tube (22) extends out of the chromatographic liquid outlet pipe (21) and is connected to an air supply pipe (26) and a liquid supply pipe (27) through a conversion valve (25); A negative pressure pump (28) is provided on the side of the chromatographic liquid outlet pipe (21); The plurality of transfer channels (10) are arranged in a stepped manner and each has a liquid inlet end, a middle section and a liquid outlet end that are sequentially connected, the liquid inlet end extends to the top wall of the transfer box (1), and the liquid outlet end extends to the bottom wall of the transfer box (1), and the middle sections of the plurality of transfer channels (10) are sequentially arranged along the thickness direction of the transfer box (1) and the projection position relationship is arranged in an array with the center of the transfer box (1) as the center of the circle; The plurality of transfer channels (10) are connected in series via a series channel (4), and the series channel (4) is provided with a series valve (41); A flow-turbulating vane (42) is provided inside the series channel (4), and the flow-turbulating vane (42) is spiral-shaped and arranged parallel to the axial direction of the series channel (4); The turbulent vane (42) is connected to the series channel (4) via a vibration spring (43).

2. The multi-channel liquid exchange device for a chromatography-mass spectrometry instrument according to claim 1, characterized in that: A transfer rack (13) is fixedly arranged between the cover plate (11) and the bottom plate (12).

3. The multi-channel liquid exchange device for a chromatography-mass spectrometry instrument according to claim 2, characterized in that: The transfer rack (13) is rotatably provided with a driving gear (14), a driving rack (15) is provided on the side wall of the transfer box (1), the driving gear (14) is meshed with the driving rack (15), and the transfer rack (13) is further provided with a transfer driving member (16) for driving the driving gear (14) to rotate.

4. The multi-channel liquid exchange device for a chromatography-mass spectrometry instrument according to claim 1, characterized in that: The cover plate (11) is connected to a flushing pipe (17), and the bottom plate (12) is connected to a recovery pipe (18).

5. The multi-channel liquid exchange device for a chromatography-mass spectrometer according to claim 1, characterized in that: The negative pressure pump (28) is connected to a filter bag (29). The bottom of the filter bag (29) is open. A plurality of gear bars (291) are arranged inside the filter bag (29), and the plurality of gear bars (291) are arranged in a staggered manner.

6. An exchange method based on the multi-channel liquid exchange device of the chromatography-mass spectrometer according to any one of claims 1 to 5, characterized in that: In the liquid supply state, the chromatographic liquid outlet pipe (21) is coaxially placed with the corresponding transfer channel (10), and the conversion valve (25) and the negative pressure pump (28) are in the closed state. In this state, the isolation plate (24) swings downward under its own gravity and enters the interior of the transfer channel (10). At this time, the bottom of the chromatographic liquid outlet pipe (21) is in the open state, and liquid supply can be carried out normally. In the non-liquid supply state, the chromatographic liquid outlet pipe (21) and the corresponding transfer channel (10) rotate relative to each other. During this process, the conversion valve (25) is adjusted to a state where the air supply pipe (26) is connected to the cleaning pipe (22), and the negative pressure pump (28) is turned on. In the process where the top wall of the transfer box (1) finally pushes the isolation plate (24) upward until the isolation plate (24) blocks the bottom of the chromatographic liquid outlet pipe (21), the negative pressure pump (28) maintains the negative pressure state inside the chromatographic liquid outlet pipe (21), and sucks the air inside the transfer channel (10) and the air inside the cleaning channel (240) and the cleaning pipe (22) from bottom to top, thereby reducing the dripping of the wall liquid in the chromatographic liquid outlet pipe (21); Before switching to connect another chromatographic liquid outlet pipe (21) with the corresponding transfer channel (10), close the conversion valve (25) and the negative pressure pump (28). After the other chromatographic liquid outlet pipe (21) is rotated to be coaxial with the corresponding transfer channel (10), the liquid supply of the other chromatographic liquid outlet pipe (21) can be realized.

Citation Information

Patent Citations

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    CN117571897B

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