Two-dimensional liquid chromatography device and system

Abstract

The utility model provides a two-dimensional liquid chromatography device and system, and in the two-dimensional liquid chromatography device, a first six-way valve, a second six-way valve and a third six-way valve are three-groove two-position six-way valves; the inlet end of the one-dimensional chromatographic column is connected with the one-dimensional liquid phase sample inlet, and the outlet end of the one-dimensional chromatographic column is connected with the No.3 position of the first six-way valve; the second position of the first six-way valve is connected with the sixth position of the third six-way valve, and the fourth position of the first six-way valve is connected with the third position of the second six-way valve; an enrichment column is connected between a first position and a fourth position of the second six-way valve, a second position of the second six-way valve is used as a waste liquid outlet, a fifth position of the second six-way valve is connected with a two-dimensional liquid phase sample inlet, and a sixth position of the second six-way valve is connected with an inlet end of a two-dimensional chromatographic column; the outlet end of the two-dimensional chromatographic column is connected with the position 2 of the third six-way valve; the first position of the third six-way valve is used for being connected with a mass spectrum detector, and the third position and the fifth position of the third six-way valve are respectively used as waste liquid outlets, so that the technical scheme that one-dimensional and two-dimensional liquid chromatograms can be connected with the mass spectrum detector is realized.

Description

Technical Field

[0001] The utility model relates to the technical field of instrument analysis, in particular to a two-dimensional liquid chromatography device and a system. Background Art

[0002] As a new type of liquid chromatography separation technology, two-dimensional liquid chromatography has better selectivity, higher resolution and analytical efficiency than one-dimensional liquid chromatography. As a powerful tool for separating complex samples, it has been widely used in fields such as pharmacy, environmental science and food science.

[0003] Since the multi-way valve plays a vital role in the connection between two dimensions and the transfer of components, it has always been regarded as a key part of multidimensional liquid chromatography. The multi-way valve is mainly composed of a circular sealing gasket (rotor) and a fixed base (stator). There are a certain number of grooves on the rotor, which play a guiding role, and each interface is fixed and located on the stator. It is used to connect the pipeline. The interfaces at both ends can be connected through the grooves, while the two ends are not connected to each other in the position without the grooves. When the multi-way valve rotates, the rotor rotates, so the position of the groove will change, and the flow direction of the mobile phase will also change accordingly. In practical applications, since there are more guide grooves on the rotor surface of the ten-way valve, eight-way valve or six-way valve, and more interfaces on the stator surface, multiple flow paths can be connected at the same time and the flow path switching can be realized, so it is widely used in the switching of multidimensional liquid chromatography. At present, the interface technology of two-dimensional chromatography is mainly divided into three types: sample loop storage technology, capture column switching technology and parallel column alternation technology. First, the quantitative loop of the sample loop storage technology is limited by the sample amount. If it is used to analyze a one-dimensional broad peak, it is necessary to cut the broad peak multiple times and finally obtain the data through multiple data splicing, which will lead to certain data errors; the capture column switching technology is to add a chromatographic column for capturing samples between the one-dimensional and two-dimensional chromatography systems, which significantly increases the amount of samples that can be collected and makes up for the shortcomings of the sample loop storage technology. However, at the same time, due to the existence of the capture column, it is necessary to consider the capture and elution methods and conditions, which will consume a certain amount of time; the parallel column alternation technology is to directly transfer to the selective second-dimensional chromatography column. The above three technologies often only connect the two-dimensional chromatography to the mass spectrometer, and lack the interface technology that connects the one-dimensional liquid phase to the mass spectrometer. When detecting mixtures with large polarity differences, there are problems of low resolution and low analysis efficiency, and it is impossible to achieve rapid separation of mixtures with large polarity differences.

[0004] Therefore, it is necessary to provide a technical solution that can achieve rapid separation of mixtures with large differences in polarity. Utility Model Content

[0005] In order to solve the above technical problems, the utility model provides a two-dimensional liquid chromatography device and system.

[0006] The utility model provides a two-dimensional liquid chromatography device, comprising: a one-dimensional chromatography column, a two-dimensional chromatography column, a first six-way valve, a second six-way valve, a third six-way valve, and an enrichment column;

[0007] The first six-way valve, the second six-way valve, and the third six-way valve are all three-slot two-position six-way valves, and the six valve ports of the three three-slot two-position six-way valves are numbered from position 1 to position 6 in a counterclockwise direction;

[0008] The inlet end of the one-dimensional chromatographic column is connected to the one-dimensional liquid phase inlet, and the outlet end thereof is connected to position 3 of the first six-way valve;

[0009] Position 2 of the first six-way valve is connected to position 6 of the third six-way valve, and position 4 thereof is connected to position 3 of the second six-way valve;

[0010] The enrichment column is connected between positions 1 and 4 of the second six-way valve, position 2 is used as a waste liquid outlet, position 5 is connected to a two-dimensional liquid phase injection port, and position 6 is connected to an inlet end of the two-dimensional chromatographic column;

[0011] The outlet end of the two-dimensional chromatographic column is connected to position 2 of the third six-way valve;

[0012] Position 1 of the third six-way valve is used to connect to a mass spectrometer detector, and positions 3 and 5 thereof are used as waste liquid outlets, respectively.

[0013] In a possible implementation, the one-dimensional chromatographic column is a hydrophilic chromatographic column.

[0014] In a possible implementation, the two-dimensional chromatography column is a reverse phase column.

[0015] The present application also provides a two-dimensional liquid chromatography system, comprising a sample injection device, the above-mentioned two-dimensional liquid chromatography device, and a mass spectrometer detector;

[0016] The sample injection device is connected to the one-dimensional liquid phase injection port and the two-dimensional liquid phase injection port respectively;

[0017] The mass spectrometer detector is connected to position 1 of the third six-way valve.

[0018] In a possible implementation, the one-dimensional chromatographic column is a hydrophilic chromatographic column.

[0019] In a possible implementation, the two-dimensional chromatography column is a reverse phase column.

[0020] The technical solution provided by the utility model has at least the following beneficial effects:

[0021] By combining three six-way valves into a flow switching device, the problem of connecting both one-dimensional and two-dimensional liquid chromatography to a mass spectrometer detector was successfully solved, which can achieve rapid detection of mixtures with large differences in polarity and improve resolution and analysis efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 A schematic diagram of a two-dimensional liquid chromatography provided by the utility model;

[0023] Figure 2 A schematic diagram of a first state of the two-dimensional liquid chromatography provided by the utility model during analysis;

[0024] Figure 3 A schematic diagram of a second state of the two-dimensional liquid chromatography provided by the utility model during analysis;

[0025] Figure 4 This is a schematic diagram of the third state of the two-dimensional liquid chromatography provided by the utility model during analysis. DETAILED DESCRIPTION

[0026] In order to deepen the understanding of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. The embodiments are only used to explain the present invention and do not limit the protection scope of the present invention.

[0027] Please refer to Figures 1 to 4 The utility model provides a two-dimensional liquid chromatography device, comprising: a one-dimensional chromatography column, a two-dimensional chromatography column, a first six-way valve, a second six-way valve, a third six-way valve, and an enrichment column;

[0028] The first six-way valve, the second six-way valve, and the third six-way valve are all three-slot two-position six-way valves, and the six valve ports of the three three-slot two-position six-way valves are numbered from position 1 to position 6 in a counterclockwise direction;

[0029] The inlet end of the one-dimensional chromatographic column is connected to the one-dimensional liquid phase inlet, and the outlet end thereof is connected to position 3 of the first six-way valve;

[0030] Position 2 of the first six-way valve is connected to position 6 of the third six-way valve, and position 4 thereof is connected to position 3 of the second six-way valve;

[0031] The enrichment column is connected between positions 1 and 4 of the second six-way valve, position 2 is used as a waste liquid outlet, position 5 is connected to a two-dimensional liquid phase injection port, and position 6 is connected to an inlet end of the two-dimensional chromatographic column;

[0032] The outlet end of the two-dimensional chromatographic column is connected to position 2 of the third six-way valve;

[0033] Position 1 of the third six-way valve is used to connect to a mass spectrometer detector, and positions 3 and 5 thereof are used as waste liquid outlets, respectively.

[0034] In the present embodiment, the one-dimensional chromatographic column and the two-dimensional chromatographic column are both conventional chromatographic columns, and the specific models can be selected according to actual needs. The first six-way valve, the second six-way valve, and the third six-way valve are all conventional six-way valves. The enrichment column adopts a conventional model. The two-dimensional liquid chromatography device, i.e., the two-dimensional liquid chromatography, includes a first dimensional separation part, a column switching device, a column enrichment part, and a second dimensional separation part. The main body of the first dimensional separation part is a one-dimensional chromatographic column, and the main body of the column switching device is three six-way valves, namely, the first six-way valve, the second six-way valve, and the third six-way valve. The waste liquid outlet can be connected to a waste liquid bottle to realize the collection of waste liquid. The one-dimensional liquid phase injection port can be connected to an injector to facilitate the operation of the one-dimensional liquid phase function. The two-dimensional liquid phase injection port can be connected to an injector to facilitate the operation of the two-dimensional liquid phase function. The one-dimensional liquid phase injection port can also input samples through an injection needle. The mass spectrometer detector is a conventional model, which can be specifically selected according to needs. The mass spectrometer detector can transmit the detection data to a computer, and the computer can record and analyze the detection data through the installed liquid chromatography software. The first six-way valve, the second six-way valve, and the third six-way valve adopt the same specifications, and all include two working states: "No. 0 working position" and "No. 1 working position". When the six-way valve is in "No. 0 working position", its No. 1 position is connected to No. 6 position, No. 2 position is connected to No. 3 position, and No. 4 position is connected to No. 5 position. When the six-way valve is in "No. 1 working position", its No. 1 position is connected to No. 2 position, No. 3 position is connected to No. 4 position, and No. 5 position is connected to No. 6 position.

[0035] In a specific embodiment, the two-dimensional liquid chromatography device first performs the first step when running, such as Figure 2 At this time, it is assumed that the first six-way valve is in "No. 1 working position", the second six-way valve is in "No. 1 working position", and the third six-way valve is in "No. 0 working position". After the mixture enters the one-dimensional chromatographic column through the one-dimensional liquid phase inlet to achieve one-dimensional liquid phase separation and retention, it enters the second six-way valve through positions 3 and 4 of the first six-way valve, enters the enrichment column through positions 3 and 4 of the second six-way valve, and then is discharged into the waste liquid (such as into a waste liquid bottle) through positions 1 and 2 of the second six-way valve; at this time, the two-dimensional liquid phase equilibrates the chromatographic column through positions 5 and 6 of the second six-way valve and positions 2 and 3 of the third six-way valve.

[0036] After executing the first step, the two-dimensional liquid chromatography device executes the second step, such as Figure 3At this time, the first six-way valve is in "No. 0 working position", the second six-way valve is in "No. 1 working position", and the third six-way valve is in "No. 0 working position". By changing the proportion of the one-dimensional liquid phase mobile phase, the components retained in the one-dimensional chromatographic column are eluted, and the eluted components pass through positions 3 and 2 of the first six-way valve and positions 6 and 1 of the third six-way valve, and enter the mass spectrometer detector for determination; at this time, the two-dimensional liquid phase is still balancing the chromatographic column through positions 5 and 6 of the second six-way valve and positions 2 and 3 of the third six-way valve.

[0037] After executing the second step, the two-dimensional liquid chromatography device executes the third step, such as Figure 4 At this time, the first six-way valve is in "No. 0 working position", the second six-way valve is in "No. 0 working position", and the third six-way valve is in "No. 1 working position". After the components retained by the one-dimensional chromatographic column are completely eluted, the one-dimensional liquid phase passes through positions 3 and 2 of the first six-way valve and positions 6 and 5 of the third six-way valve, and is discharged into the waste liquid (such as into the waste liquid bottle); at this time, the two-dimensional liquid phase is connected to the enrichment column through positions 5 and 4 of the second six-way valve, and then through positions 1 and 6. After being retained and separated by the two-dimensional chromatographic column, it is connected to the mass spectrometer detector through positions 2 and 1 of the third six-way valve for determination. After all the components in the enrichment column are eluted and determined, the analysis process ends.

[0038] In a possible implementation, the one-dimensional chromatographic column is a hydrophilic chromatographic column.

[0039] In a possible implementation, the two-dimensional chromatography column is a reverse phase column.

[0040] In this embodiment, one-dimensional liquid phase and two-dimensional liquid phase can be realized by connecting chromatographic columns with different separation mechanisms, so as to achieve higher analysis efficiency. For example, a hydrophilic chromatography (HILIC) column, i.e., a one-dimensional chromatographic column, is connected to a one-dimensional liquid phase, and a reverse phase chromatography (RPC) column, i.e., a two-dimensional chromatographic column, is connected to a two-dimensional liquid phase, so as to achieve rapid separation of mixtures with large differences in polarity.

[0041] The present application also provides a two-dimensional liquid chromatography system, comprising a sample injection device, the above-mentioned two-dimensional liquid chromatography device, and a mass spectrometer detector;

[0042] The sample injection device is connected to the one-dimensional liquid phase injection port and the two-dimensional liquid phase injection port respectively;

[0043] The mass spectrometer detector is connected to position 1 of the third six-way valve.

[0044] In a possible implementation, the one-dimensional chromatographic column is a hydrophilic chromatographic column.

[0045] In a possible implementation, the two-dimensional chromatography column is a reverse phase column.

[0046] The above embodiments should not limit the present invention in any way, and any technical solutions obtained by equivalent replacement or equivalent conversion shall fall within the protection scope of the present invention.

Claims

1. A two-dimensional liquid chromatography device, characterized in that: include: A one-dimensional chromatographic column, a two-dimensional chromatographic column, a first six-way valve, a second six-way valve, a third six-way valve, and an enrichment column; The first six-way valve, the second six-way valve, and the third six-way valve are all three-slot two-position six-way valves, and the six valve ports of the three three-slot two-position six-way valves are numbered from position 1 to position 6 in a counterclockwise direction; The inlet end of the one-dimensional chromatographic column is connected to the one-dimensional liquid phase inlet, and the outlet end thereof is connected to position 3 of the first six-way valve; Position 2 of the first six-way valve is connected to position 6 of the third six-way valve, and position 4 thereof is connected to position 3 of the second six-way valve; The enrichment column is connected between positions 1 and 4 of the second six-way valve, position 2 is used as a waste liquid outlet, position 5 is connected to a two-dimensional liquid phase injection port, and position 6 is connected to an inlet end of the two-dimensional chromatographic column; The outlet end of the two-dimensional chromatographic column is connected to position 2 of the third six-way valve; Position 1 of the third six-way valve is used to connect to a mass spectrometer detector, and positions 3 and 5 thereof are used as waste liquid outlets, respectively.

2. The two-dimensional liquid chromatography device according to claim 1, characterized in that: The one-dimensional chromatographic column is a hydrophilic chromatographic column.

3. The two-dimensional liquid chromatography device according to claim 1, characterized in that: The two-dimensional chromatographic column is a reverse phase column.

4. A two-dimensional liquid chromatography system, characterized in that: It comprises a sample injection device, a two-dimensional liquid chromatography device as claimed in claim 1, and a mass spectrometer detector; The sample injection device is connected to the one-dimensional liquid phase injection port and the two-dimensional liquid phase injection port respectively; The mass spectrometer detector is connected to position 1 of the third six-way valve.

5. The two-dimensional liquid chromatography system according to claim 4, characterized in that: The one-dimensional chromatographic column is a hydrophilic chromatographic column.

6. The two-dimensional liquid chromatography system according to claim 4, characterized in that: The two-dimensional chromatographic column is a reverse phase column.

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