Multi-mode automatic switching continuous sampling device of liquid chromatograph-mass spectrometer

By introducing a multi-mode automatic switching continuous injection device into the liquid chromatography-mass spectrometry (LC-MS) system, the cumbersome operation problem of switching separation modes and detectors in LC-MS has been solved, realizing the automation of high-throughput continuous injection and improving operational efficiency and instrument utilization.

CN223692336UActive Publication Date: 2025-12-19DALIAN UNIV OF TECH
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Patent Information

Application Number
CN202423221080.1
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-12-25
Publication Date
2025-12-19
Estimated Expiration
2034-12-25

AI Technical Summary

Technical Problem

Liquid chromatography-mass spectrometry (LC-MS) instruments are cumbersome to operate when switching between different separation modes and detectors, which can easily wear out parts. Furthermore, sample detection in different modes requires separate settings, making it impossible to achieve automated, high-throughput, continuous sample injection.

Method used

A multi-mode automatic switching continuous injection device is adopted, including switching valves A, B, and C. Through the connection between the liquid chromatography pump system and the mass spectrometry system, the automatic switching between reversed-phase chromatography-mass spectrometry, hydrophilic interaction chromatography-mass spectrometry, and reversed-phase chromatography-ultraviolet-mass spectrometry is realized. High-throughput continuous injection is achieved by using the liquid chromatography-mass spectrometry control system.

Benefits of technology

It eliminates the need for frequent column and detector replacements, improving operational efficiency and instrument utilization, and enabling automatic switching between different modes and high-throughput continuous injection.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model provides a multi-mode automatic switching continuous sampling device of a liquid chromatograph-mass spectrometer, which relates to the technical field of scientific instruments and comprises three switching valves. A sample inlet of the switching valve A is connected with the liquid chromatography pump system, a sample outlet of the switching valve A is connected with an inlet of the first chromatographic column, and an outlet of the first chromatographic column is connected with a first sample inlet of the switching valve B; another sample outlet of the switching valve A is connected with an inlet of a second chromatographic column, and an outlet of the second chromatographic column is connected with a second sample inlet of the switching valve B; a first outlet of the switching valve B is connected with a first inlet of the switching valve C, and a second outlet of the switching valve B is connected with a second inlet of the switching valve C; and an outlet of the switching valve C is connected with a sample inlet of the mass spectrum system. According to the utility model, the three modes of first chromatographic column-mass spectrum, second chromatographic column-mass spectrum and second chromatographic column-ultraviolet-mass spectrum can be detected under the same acquisition instruction, so that the working efficiency of operators and the utilization rate of mass spectrometers are improved.
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Description

TECHNICAL FIELD

[0001] The utility model relates to scientific instrument technical field especially, relate to a kind of multimode automatic switching continuous sample introduction device of liquid quality combination appearance. BACKGROUND

[0002] Liquid chromatography-mass spectrometry is an important separation and analysis technology, and is an essential means and tool for research in chemical engineering, biomedicine, material science and environmental science. Mass spectrometry as a detection unit can provide mass-to-charge ratio information of molecules and fragments. Liquid chromatography is the separation unit and sample introduction unit of mass spectrometry, and the liquid chromatography column is the core of liquid chromatography separation, which determines the effect and efficiency of sample separation. Common chromatographic separation modes include reversed-phase chromatography, normal-phase chromatography, hydrophobic interaction chromatography, hydrophilic interaction chromatography and ion exchange chromatography, etc.

[0003] Liquid chromatography-mass spectrometry is a large instrument sharing management system, and the samples come from chemistry, chemical engineering, environment, biological engineering, electrical engineering, materials and transportation disciplines, and the sample structure is diverse. Liquid chromatography is the separation unit at the front end of mass spectrometry, and a unified separation mode cannot be used to complete the sample test in a day. According to the characteristics of the compounds, the reversed-phase mode and the hydrophilic mode need to be frequently switched in daily liquid quality test, and the reversed-phase chromatography needs to be frequently switched between whether to connect the ultraviolet detector. The instrument operator needs to detect complex system samples with different components every day, and there are the following disadvantages when changing the automatic sample introduction mode and whether to connect the ultraviolet detector: (1) the chromatography column needs to be frequently replaced, and whether to connect the ultraviolet detector needs to be selected, which is relatively cumbersome to operate; (2) the pipeline interface is easy to be not tightened, causing liquid leakage; (3) due to frequent replacement, the pipeline interface is easy to be damaged, causing accessory loss; (4) when changing the separation mode, manual conversion is needed, which is not conducive to automatic switching of liquid phase mode at night or on weekends; (5) different modes of separated samples cannot be detected simultaneously, and sampling programs need to be set separately. Utility model content

[0004] The utility model provides a multimode automatic switching continuous sample introduction device of liquid quality combination appearance, realize reversed-phase chromatography mode automatic switching connection ultraviolet detector's high throughput continuous sample introduction device, reach the purpose of continuous automatic sample introduction using the autosampler in liquid chromatograph.

[0005] To achieve the above purpose, the technical scheme adopted by the utility model is as follows:

[0006] A multimode automatic switching continuous sample introduction device of liquid quality combination appearance, comprising a switching valve A, a switching valve B and a switching valve C.

[0007] The sample inlet of the switching valve A is connected with a liquid chromatograph pump system, one sample outlet of the switching valve A is connected with a first chromatographic column inlet, and the first chromatographic column outlet is connected with a first sample inlet of a switching valve B; another sample outlet of the switching valve A is connected with a second chromatographic column inlet, and the second chromatographic column outlet is connected with a second sample inlet of the switching valve B;

[0008] The first outlet of the switching valve B is connected with a first inlet of a switching valve C, and the second outlet of the switching valve B is connected with a second inlet of the switching valve C.

[0009] The outlet of the switching valve C is connected with a sample inlet of a mass spectrometer system.

[0010] Further, the switching valve A, the switching valve B and the switching valve C are electrically connected with a control system of the liquid chromatograph-mass spectrometer.

[0011] Further, the second outlet of the switching valve B is connected with the second inlet of the switching valve C through a pipeline after passing through an ultraviolet detector.

[0012] Further, the liquid chromatograph-mass spectrometer comprises a liquid chromatograph and a mass spectrometer system, the liquid chromatograph comprises a liquid chromatograph pump system, an automatic sample injector, an ultraviolet detector and a column oven module, and a chromatographic column is arranged in the column oven module.

[0013] Further, the chromatographic column comprises a first chromatographic column and a second chromatographic column, the column oven system of the liquid chromatograph is provided with the switching valve A and the switching valve B, and the front end of the mass spectrometer system is provided with the switching valve C.

[0014] Further, the switching valve A, the switching valve B and the switching valve C comprise a 6-position 2-way switching valve, a 10-position 2-way switching valve or a 10-position 4-way switching valve.

[0015] Further, the first chromatographic column and the second chromatographic column are chromatographic columns of the same or different separation modes or two ways.

[0016] The utility model discloses the beneficial effect lies in:

[0017] The utility model discloses the program of having dispensed with frequently replacing chromatographic column and whether connecting ultraviolet detector, can realize that the first chromatographic column / two -way - mass spectrometer, second chromatographic column - mass spectrometer and second chromatographic column - ultraviolet - mass spectrometer three modes complete detection under the same acquisition instruction, greatly improve the work efficiency of operating personnel and the use ratio of mass spectrometer instrument.

[0018] The utility model discloses a structure for the automatic switching of the two kinds of sample injection modes of the reversed phase chromatography-mass spectrometry and the hydrophilic interaction chromatography-mass spectrometry, and the reversed phase chromatography-ultraviolet-mass spectrometry, and realizes the high-throughput continuous sample injection. BRIEF DESCRIPTION OF DRAWINGS

[0019] In order to more clearly illustrate the embodiments of the utility model or the technical solutions of the prior art, the drawings needed to be used in the embodiment or the prior art description will be simply introduced below, and obviously, the drawings in the following description are only some embodiments of the utility model, and for the ordinary skilled in the art, other drawings can also be obtained according to these drawings without creative labor.

[0020] Figure 1 It is the structure schematic drawing that the utility model sample injection device switches to the first chromatographic column / two - way - mass spectrum mode.

[0021] Figure 2 It is the structure schematic drawing that the utility model sample injection device switches to the second chromatographic column - mass spectrum mode.

[0022] Figure 3 It is the structure schematic drawing that the utility model sample injection device switches to the second chromatographic column - ultraviolet - mass spectrum mode.

[0023] BRIEF DESCRIPTION OF DRAWINGS

[0024] 1, switching valve A;2, switching valve B;3, switching valve C;4, liquid chromatograph pump system;5, mass spectrometry system;6, ultraviolet detector;7, column oven module;8, first chromatographic column;9, second chromatographic column. DETAILED DESCRIPTION

[0025] It should be noted that the embodiments in the utility model and the features in the embodiments can be combined with each other without conflict. The utility model will be described in detail below with reference to the drawings and in combination with the embodiments.

[0026] In order to make the purpose, technical scheme and advantages of the embodiments of the utility model clearer, the technical scheme in the embodiments of the utility model will be described clearly and completely in combination with the drawings in the embodiments of the utility model below. Obviously, the described embodiments are only part of the embodiments of the utility model, rather than all the embodiments. The description of the at least one exemplary embodiment is actually only illustrative, but not as any limitation on the utility model and its application or use. Based on the embodiments in the utility model, all other embodiments obtained by those skilled in the art without creative labor belong to the protection scope of the utility model.

[0027] It should be noted that the terms used herein are only for describing specific embodiments, and are not intended to limit the exemplary embodiments according to the utility model. As used herein, the singular form is intended to include the plural form unless the context clearly indicates otherwise, and furthermore, it should be understood that when the terms "comprise" and / or "include" are used in the specification, there is a feature, step, operation, device, component and / or combination thereof.

[0028] Unless specifically stated otherwise, the relative arrangement of components and steps, numerical expressions, and numerical values set forth in the embodiments are not intended to limit the scope of the utility model. At the same time, it should be clear that the sizes of the various parts shown in the drawings are not drawn in proportion to the actual proportions. The technology, methods and devices known to those skilled in the relevant art may not be discussed in detail, but in appropriate cases, the technology, methods and devices should be considered as part of the authorized specification. In all examples shown and discussed herein, any specific value should be interpreted as merely exemplary, and not as a limitation. Therefore, other examples of exemplary embodiments can have different values. It should be noted that similar reference numbers and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further discussed in subsequent drawings.

[0029] In addition, it should be noted that the use of "first", "second" and the like to define parts is only for the convenience of distinguishing the corresponding parts, and the above words have no special meaning unless otherwise stated, so they cannot be understood as limiting the protection scope of the utility model.

[0030] The utility model provides a kind of technical scheme: a multimode automatic switching continuous sample introduction device of liquid chromatograph-mass spectrometer, such as Figure 1As shown, this is used in a liquid chromatography-mass spectrometry (LC-MS) system. Taking a Thermo Fisher Scientific LC-MS system as an example, the LC-MS system includes a liquid chromatograph (LC) and a mass spectrometry (MS) system 5. The LC includes a liquid chromatography pump system 4, an autosampler, a UV detector 6, and a column oven. The column oven contains a chromatographic column. The automatic switching high-throughput continuous injection device includes switching valves A1, B2, and C3. The inlet of switching valve A1 is connected to the LC pump of the LC. One outlet of switching valve A1 is connected to the inlet of the hydrophilic interaction column in the LC column oven, and the outlet of the hydrophilic interaction column is connected to the inlet of switching valve B2. The other outlet of switching valve A1 is connected to the inlet of the reversed-phase column in the LC column oven, and the outlet of the reversed-phase column is connected to the other inlet of switching valve B2. One outlet of switching valve B2 is connected to the inlet of switching valve C3, and the other outlet of switching valve B2, after passing through the UV detector 6, is connected to the other inlet of switching valve C3 via a tubing. The outlet of switching valve C3 is connected to the inlet of mass spectrometry system 5, and the switching valve is electrically connected to the control system of liquid chromatography-mass spectrometry instrument.

[0031] An ultraviolet detector 6 is installed on the pipeline between the other outlet of switching valve B2 and the other inlet of switching valve C3.

[0032] The switching valves include 6-position 2-way switching valves, 10-position 2-way switching valves, or 10-position 4-way switching valves.

[0033] like Figure 1 As shown, the 1>2, 1>2, and 1>6 passages of the switching valve are connected;

[0034] like Figure 2 As shown, the 1>6, 1>6, and 1>6 passages of the switching valve are connected;

[0035] like Figure 3 As shown, the 1>6, 1>2, and 1>2 passages of the switching valve are connected.

[0036] This embodiment provides an automatic high-throughput continuous injection device for use in a liquid chromatography-mass spectrometry (LC-MS) system, supporting three modes: first column 8 / two-way port-mass spectrometry, second column 9-mass spectrometry, and second column 9 UV-mass spectrometry. The device includes switching valves A1 and B2 mounted on the LC column oven module 7, and a switching valve C3 for the mass spectrometer front-end. The LC-MS system is an existing instrument comprising a liquid chromatograph and a mass spectrometry system 5. The liquid chromatograph includes a liquid chromatography pump and a column oven, which houses the first column 8 / two-way port and the second column 9.

[0037] Example 1:

[0038] The switching valve A1, B2, C3 adopts a 6-position 2-way column switching valve of Thermo Fisher Corporation, wherein 1, 3, 5 ports are sample inlet ports, and 2, 4, 6 ports are sample outlet ports; the sample inlet port (1 port) of the switching valve A1 is connected with the pump system of the liquid chromatograph through a pipeline; one sample outlet port (2 port) of the switching valve A1 is connected with the two-way inlet of the first chromatographic column 8 through a pipeline; the two-way outlet of the first chromatographic column 8 is connected with the sample inlet port (5 port) of the switching valve B2 through a pipeline; one sample outlet port (6 port) of the switching valve B2 is connected with one sample inlet port (3 port) of the switching valve C3 through a pipeline; one sample outlet port (2 port) of the switching valve C3 is connected with the mass spectrometer through a pipeline; the other sample outlet port (6 port) of the switching valve A1 is connected with the inlet of the second chromatographic column 9 through a pipeline; the outlet of the second chromatographic column 9 is connected with the sample inlet port (1 port) of the switching valve B2 through a pipeline; one sample outlet port (6 port) of the switching valve B2 is connected with one sample inlet port (3 port) of the switching valve C3 through a pipeline; one sample outlet port (2 port) of the switching valve C3 is connected with the mass spectrometer through a pipeline; the other sample outlet port (6 port) of the switching valve A1 is connected with the inlet of the second chromatographic column 9 through a pipeline; the outlet of the second chromatographic column 9 is connected with the sample inlet port (1 port) of the switching valve B2 through a pipeline; the other sample outlet port (2 port) of the switching valve B2 is connected with the ultraviolet detector 6 through a pipeline; after passing through the ultraviolet detector 6, the pipeline is connected with the other sample inlet port (1 port) of the switching valve C3; one sample outlet port (2 port) of the switching valve C3 is connected with the mass spectrometer through a pipeline; the column switching valves A1, B2 and C3 are electrically connected with the control system of the liquid chromatograph-mass spectrometer.

[0039] The first chromatographic column 8 / two-way-mass spectrometer, the second chromatographic column 9-mass spectrometer and the second chromatographic column 9-ultraviolet-mass spectrometer mode automatic switching high-throughput continuous sampling device of the utility model, its specific operation mode is mainly divided into the following points:

[0040] 1) connect the required pipeline and passage, so that when the 6-position 2-way column switching valve A1, B2, C3 is connected with 1>2, 1>2, 1>6 passage respectively, the system is the first chromatographic column 8 / two-way-mass spectrometer mode; when the 6-position 2-way column switching valve is connected with 1>6, 1>6, 1>6 passage respectively, the system is the second chromatographic column 9-mass spectrometer mode; when the 6-position 2-way column switching valve is connected with 1>6, 1>2, 1>2 passage respectively, the system is the second chromatographic column 9-ultraviolet-mass spectrometer mode;

[0041] 2) the function module (for product self-owned) of the 6-position 2-way column switching valve is driven through the liquid chromatograph-mass spectrometer control system, so that the control system can realize one-key control of the automatic switching of the first chromatographic column 8 / two-way-mass spectrometer, the second chromatographic column 9-mass spectrometer and the second chromatographic column 9-ultraviolet-mass spectrometer mode;

[0042] 3) In the control system, set the method of liquid chromatography collection and the method of mass spectrometry collection in three modes of first chromatographic column 8 / two-way-mass spectrometry, second chromatographic column 9-mass spectrometry and second chromatographic column 9-ultraviolet-mass spectrometry mode respectively, wherein, when the second chromatographic column 9-ultraviolet-mass spectrometry mode needs to use the ultraviolet detector 6, the flow rate and the solvent ratio of the liquid chromatography can be set according to the requirement, at the same time, in the first chromatographic column 8 / two-way-mass spectrometry mode, the connection mode of the column switching valve A1-C3 is set to 1>2, 1>2, 1>6, in the second chromatographic column 9-mass spectrometry mode, the connection mode of the column switching valve A1-C3 is set to 1>6, 1>6, 1>6, in the second chromatographic column 9-ultraviolet-mass spectrometry mode, the connection mode of the column switching valve A1-C3 is set to 1>6, 1>2, 1>2;

[0043] 4) In the control system, edit the sample table (sequence) of the liquid chromatography-mass spectrometry instrument, set the information and method of the samples of the first chromatographic column 8 / two-way-mass spectrometry, the second chromatographic column 9-mass spectrometry and the second chromatographic column 9-ultraviolet-mass spectrometry mode, so that the three modes of the first chromatographic column 8 / two-way-mass spectrometry, the second chromatographic column 9-mass spectrometry and the second chromatographic column 9-ultraviolet-mass spectrometry can realize automatic switching and complete detection under the same collection instruction (sequence).

[0044] The above only describes the preferred embodiments of the present application, and the protection scope of the present application is not limited to this. Any skilled person in the art can make equivalent replacement or change according to the technical scheme and the inventive concept of the present application within the technical range disclosed by the present application, which should be covered in the protection scope of the present application.

Claims

1. A multi-mode automatic switching continuous sample introduction device for liquid chromatography-mass spectrometry, characterized in that, The switching valve A (1), the switching valve B (2) and the switching valve C (3) are connected with the control system of the liquid chromatograph-mass spectrometer. The sample inlet of the switching valve A (1) is connected with the liquid chromatograph pump system (4), one sample outlet of the switching valve A (1) is connected with the inlet of the first chromatographic column (8), the outlet of the first chromatographic column (8) is connected with the first sample inlet of the switching valve B (2); the other sample outlet of the switching valve A (1) is connected with the inlet of the second chromatographic column (9), the outlet of the second chromatographic column (9) is connected with the second sample inlet of the switching valve B (2). The first outlet of the switching valve B (2) is connected with the first inlet of the switching valve C (3), the second outlet of the switching valve B (2) is connected with the second inlet of the switching valve C (3). The outlet of the switching valve C (3) is connected with the sample inlet of the mass spectrometer system (5).

2. The multi-mode automatic switching continuous sample introduction device for liquid chromatograph-mass spectrometer of claim 1, wherein, The switching valve A (1), the switching valve B (2) and the switching valve C (3) are electrically connected with the control system of the liquid chromatograph-mass spectrometer.

3. The multi-mode automatic switching continuous sample introduction device for liquid chromatograph-mass spectrometer of claim 1, wherein, The second outlet of the switching valve B (2) is connected with the second inlet of the switching valve C (3) through the pipeline after passing through the ultraviolet detector (6).

4. The multi-mode automatic switching continuous sample introduction device for liquid chromatograph-mass spectrometer of claim 1, wherein, The liquid chromatograph-mass spectrometer comprises a liquid chromatograph and a mass spectrometer system (5), the liquid chromatograph comprises a liquid chromatograph pump system (4), an automatic sampler, an ultraviolet detector (6) and a column oven module (7), and the column oven module (7) is provided with chromatographic columns.

5. The multi-mode automatic switching continuous sample introduction device for liquid chromatograph-mass spectrometer of claim 4, wherein, The chromatographic columns comprise a first chromatographic column (8) and a second chromatographic column (9), the column oven system of the liquid chromatograph is provided with the switching valve A (1) and the switching valve B (2), and the front end of the mass spectrometer system (5) is provided with the switching valve C (3).

6. The multi-mode automatic switching continuous sample introduction device for liquid chromatograph-mass spectrometer of claim 1, wherein, The switching valve A (1), the switching valve B (2) and the switching valve C (3) comprise a 6-position 2-way switching valve, a 10-position 2-way switching valve or a 10-position 4-way switching valve.

7. The multi-mode automatic switching continuous sample introduction device for liquid chromatograph-mass spectrometer of claim 1, wherein, The first chromatographic column (8) and the second chromatographic column (9) are chromatographic columns of the same or different separation modes or two-way chromatographic columns. The first chromatographic column (8) and the second chromatographic column (9) are chromatographic columns of the same or different separation modes or two-way chromatographic columns.