JP6672781B2 - Flow path mechanism and liquid chromatograph provided with the same - Google Patents

Description

  The present invention relates to a channel mechanism for separating a sample component in a solvent and detecting the sample component with a detector, and a liquid chromatograph provided with the channel mechanism.

  In liquid chromatography, when multiple types of solvents are mixed by a mixer and the mixed solvent is sent as a mobile phase to a separation column, sample components in the solvent are separated by a separation column for analysis. There is. In such an analysis, the solvent may be sent at different flow rates such as a flow rate (conventional flow rate) of about 50 μL / min to 1 mL / min or a flow rate (micro flow rate) of 50 μL / min or less. Usually, such a liquid chromatograph is provided with one mixer.

  Patent Literature 1 below discloses a liquid chromatograph including a conventional mixer used when sending a solvent at a conventional flow rate and a micromixer used when sending a solvent at a micro flow rate. In this example, the solvent is sent at a conventional flow rate using a conventional mixer during normal analysis, and the solvent is sent at a micro flow rate using a micro mixer during concentration analysis. That is, Patent Document 1 discloses a configuration in which a plurality of types of mixers having different capacities are switched and used.

Japanese Patent No. 5012148

  However, in the above-described conventional configuration, when replacing a separation column according to analysis conditions, an operator must manually remove the separation column and attach another separation column. For this reason, apart from switching a plurality of types of mixers, it is necessary to exchange the separation column, and the operation when performing analysis with different internal volumes is complicated.

  The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a flow channel mechanism that facilitates work when performing analysis with different internal capacities, and a liquid chromatograph including the same.

  The flow path mechanism according to the present invention is a flow path mechanism for separating a sample component in a solvent and detecting the sample component with a detector, and includes a first mixer, a second mixer, a first separation column, A separation column and a flow path switching unit are provided. The first mixer mixes a solvent therein. The second mixer has a different capacity from the first mixer, and internally mixes a solvent. The first separation column is associated with the first mixer. The second separation column is associated with the second mixer. The flow path switching unit may be a first communication state in which the first mixer and the first separation column communicate with the detector, or a second communication state in which the second mixer and the second separation column communicate with the detector. Switch to the communication state.

  According to such a configuration, the first mixer and the first separation column are connected to the detector using the flow path switching unit, or the second mixer and the second separation column are connected to the detector. It can be easily switched to the second communication state. As described above, by simply switching the flow path switching unit, it is possible to easily switch to the first communication state or the second communication state in which the internal capacity of the flow path is different, so that the work when performing analysis with a different internal capacity is easy. It is.

  The channel mechanism may further include a column oven. The column oven contains the first mixer, the second mixer, the first separation column, and the second separation column, and the inside is heated.

  According to such a configuration, the first mixer, the second mixer, the first separation column, and the second separation column are all housed in the column oven. Therefore, the operation of exchanging the mixer and the operation of exchanging the separation column can be performed at the same time, which further facilitates the operation.

  The flow path switching unit may be constituted by one valve.

  According to such a configuration, it is possible to easily switch to the first communication state or the second communication state in which the internal capacity of the flow path is different by simply switching one valve. Thus, there is no need to synchronize the switching timing as in the case of switching a plurality of valves, so that the operation is further facilitated.

  The channel mechanism may further include a concentration column that captures and concentrates the sample. In this case, in the first communication state, the sample concentrated in the concentration column is led to the first separation column, and in the second communication state, the sample concentrated in the concentration column is separated into the second separation column. It may be led to a column.

  According to such a configuration, the sample captured and concentrated in the concentration column can be selectively guided to the first separation column or the second separation column only by switching the flow path switching unit. Therefore, by easily switching to the first communication state or the second communication state in which the internal volume of the flow path is different, and guiding the concentrated sample to the first separation column or the second separation column, any one of the separation columns is used. Analysis can be performed well.

  A liquid chromatograph according to the present invention includes the flow path mechanism and a detector. The detector detects a sample component in the solvent separated by the first separation column in the first communication state, or a sample component in the solvent separated by the second separation column in the second communication state. I do.

  According to the present invention, it is possible to easily switch to the first communication state or the second communication state in which the internal capacity of the flow path is different simply by switching the flow path switching unit. Is easy.

FIG. 1 is a flow chart illustrating a configuration example of a liquid chromatograph according to an embodiment of the present invention. FIG. 2 is a flow chart showing a state where a second valve is rotated from the state of FIG. 1. FIG. 2 is a flow chart illustrating a state in which a first valve is rotated from the state of FIG. FIG. 4 is a flow chart showing a state where a second valve is rotated from the state shown in FIG. 3.

  FIG. 1 is a flow chart showing a configuration example of a liquid chromatograph according to one embodiment of the present invention. This liquid chromatograph includes a plurality of containers 1, a degassing unit 2, a low-pressure gradient unit 3, a liquid-feeding pump 4, a column oven 5, an autosampler 6, a detector 7, and the like, and can perform low-pressure gradient analysis. it can.

  Each of the plurality of containers 1 contains a different type of solvent. These solvents are sent out from each container 1 as a mobile phase by driving the liquid sending pump 4. The plurality of types of solvents sent from each container 1 are degassed by passing through the degassing unit 2 and then join at a constant ratio in the low-pressure gradient unit 3. The mixing ratio of each solvent can be adjusted in the low-pressure gradient unit 3.

  The column oven 5 is partitioned by a hollow housing (not shown), and includes therein a first mixer 51, a second mixer 52, a first separation column 53, a second separation column 54, a first valve 55, and the like. Is housed. The first mixer 51, the second mixer 52, the first separation column 53, and the second separation column 54 are respectively connected to the first valve 55 via a pipe. A heater (not shown) is arranged in the column oven 5, and the inside of the column oven 5 is heated by the heater.

  The plurality of types of solvents that have joined in the low-pressure gradient unit 3 are guided into the column oven 5 via the liquid sending pump 4, and flow into either the first mixer 51 or the second mixer 52. In the state shown in FIG. 1, a plurality of types of solvents flow into the first mixer 51. However, when the first valve 55 is rotated, a plurality of types of solvents flow into the second mixer 52. State.

  The autosampler 6 includes a needle 61, a syringe 62, a concentration column 63, a second valve 64, and the like. The needle 61 is inserted into a sample container (not shown) and aspirates a sample from inside the sample container. The syringe 62 is driven when sucking a sample from the needle 61.

  The concentration column 63 is a so-called sample loop, and communicates with the needle 61. In the state of FIG. 1, the needle 61 communicates with the syringe 62 via the concentration column 63. In this state, when the syringe 62 is driven to suck the sample from the needle 61, the sucked sample is captured by the concentration column 63 and concentrated in the concentration column 63. Thereafter, the needle 61 is inserted into the sample introduction section 65 communicating with the second valve 64, and the second valve 64 is rotated, so that a plurality of types of solvents mixed by the first mixer 51 or the second mixer 52 are concentrated. Go through 63. As a result, the sample is introduced into a plurality of types of mixed solvents, and the sample is guided to the first separation column 53 or the second separation column 54 in the column oven 5.

  The second valve 64 is composed of, for example, a six-port valve having six ports a to f. A syringe 62 communicates with a port a of the second valve 64 via a pipe, and a needle 61 communicates with a port f via a pipe and a concentration column 63. The sample introduction part 65 is connected to the port c of the second valve 64 via a pipe. The ports d and e of the second valve 64 communicate with the first valve 55 in the column oven 5 via piping. The port b of the second valve 64 communicates with a drain (not shown).

  The first valve 55 includes, for example, a 10-port valve having ten ports a to j. The inlets and outlets of the first mixer 51 communicate with the ports a and b of the first valve 55 via pipes, respectively, and the inlets and outlets of the second mixer 52 connect with the ports i and d, respectively. It communicates via piping. The port g of the first valve 55 communicates with the upstream end of the first separation column 53 via a pipe, and the port e communicates with the upstream end of the second separation column 54 via a pipe. The ports c and f of the first valve 55 communicate with the second valve 64 of the autosampler 6 via a pipe. The port j of the first valve 55 communicates with the liquid feed pump 4 via a pipe. A pipe is connected to the port h of the first valve 55, and the end of the pipe is closed by a stop joint (not shown).

  The first mixer 51 is a gradient mixer having a relatively small capacity. More specifically, the volume of the solvent is less than 100 μL (for example, 40 μL), and a plurality of types of the inflowing solvents are mixed by repeating the branching and merging of the flow path formed therein. The first mixer 51 is associated with a first separation column 53.

  The second mixer 52 is a gradient mixer having a relatively large capacity, and has a capacity different from that of the first mixer 51. More specifically, the volume of the solvent is 100 μL or more (for example, 750 μL), and a plurality of types of the inflowing solvents are mixed by repeating the branching and merging of the flow path formed therein. The second separation column 54 is associated with the second mixer 52.

  The first separation column 53 and the second separation column 54 join on the downstream side via a manifold 56, and the manifold 56 is connected to the detector 7 via a pipe. The detector 7 includes a cell 71, a light source 72, and a light receiving unit 73. The sample that has passed through the first separation column 53 or the second separation column 54 is led into the cell 71 of the detector 7. The cell 71 is irradiated with measurement light from a light source 72, and the measurement light transmitted through the cell 71 is received by a light receiving unit 73. Since the measurement light transmitted through the cell 71 is absorbed at a wavelength unique to the sample in the cell 71, the sample can be identified based on the intensity of the measurement light received by the light receiving unit 73.

  In the state of FIG. 1, the ports a and j of the first valve 55 are connected, and the ports b and c are connected. Therefore, the plurality of types of solvents flowing from the liquid sending pump 4 to the port j of the first valve 55 are mixed in the first mixer 51 and then flow to the port e of the second valve 64. In the second valve 64, ports d and e are in communication. Therefore, the plurality of types of solvents mixed in the first mixer 51 pass through the second valve 64 without flowing into the concentration column 63, and flow into the port f of the first valve 55.

  In the first valve 55, ports f and g are in communication. Therefore, the mixed plural kinds of solvents are guided to the first separation column 53, and after flowing through the first separation column 53, flow into the cell 71 of the detector 7. As described above, in the state of FIG. 1, the plurality of types of solvents mixed in the first mixer 51 are guided to the first separation column 53 without introducing a sample.

  In the state of FIG. 1, the ports a and f of the second valve 64 are in communication. Therefore, if the syringe 62 is driven in this state and the sample is sucked from the needle 61, the sample can be captured in the concentration column 63 and concentrated. When the sample is analyzed using the first mixer 51 and the first separation column 53, the needle is inserted into the sample introduction section 65 after the sample is captured in the concentration column 63 in this manner, and the second valve 64 will be rotated.

  FIG. 2 is a flow chart showing a state where the second valve 64 is rotated from the state of FIG. In the state of FIG. 2, the ports c and d of the second valve 64 communicate with each other, and the ports e and f communicate with each other. Therefore, the plurality of types of solvents mixed in the first mixer 51 do not pass directly to the first separation column 53 as in the case of FIG. 1 but pass through the concentration column 63 and enter into the concentration column 63. After the concentrated sample is introduced, it is led to the first separation column 53.

  The sample thus introduced into the first separation column 53 is separated for each sample component while passing through the first separation column 53, and is led to the cell 71 of the detector 7. Then, the measurement light from the light source 72 transmitted through the cell 71 is received by the light receiving unit 73, and the peak of each separated sample component is detected based on the received light intensity. Thus, high-speed analysis can be performed by analyzing a sample using the first separation column 53 using a plurality of types of solvents mixed in the first mixer 51 as a mobile phase.

  FIG. 3 is a flow chart showing a state where the first valve 55 is rotated from the state shown in FIG. In the state of FIG. 3, the second valve 64 is in the same state as in FIG. 1, and the ports a and f of the second valve 64 are in communication. Therefore, if the syringe 62 is driven in this state and the sample is sucked from the needle 61, the sample can be captured in the concentration column 63 and concentrated.

  In the state of FIG. 3, the ports c and d of the first valve 55 communicate with each other, and the ports i and j communicate with each other. Therefore, the plurality of types of solvents flowing from the liquid feed pump 4 to the port j of the first valve 55 are mixed in the second mixer 52 and then flow to the port e of the second valve 64. In the second valve 64, ports d and e are in communication. Therefore, the plurality of types of solvents mixed in the second mixer 52 pass through the second valve 64 without flowing into the concentration column 63, and flow into the port f of the first valve 55.

  In the first valve 55, ports e and f are in communication. Therefore, the mixed plural kinds of solvents are guided to the second separation column 54, and after flowing through the second separation column 54, flow into the cell 71 of the detector 7. Thus, in the state of FIG. 3, the plurality of types of solvents mixed in the second mixer 52 are led to the second separation column 54 without introducing a sample. When a sample is analyzed using the second mixer 52 and the second separation column 54, after capturing the sample in the concentration column 63 in such a state, the needle 61 is inserted into the sample introduction unit 65, and the second The valve 64 will be rotated.

  FIG. 4 is a flow chart showing a state where the second valve 64 is rotated from the state of FIG. In the state of FIG. 4, the ports c and d of the second valve 64 communicate with each other, and the ports e and f communicate with each other. Therefore, the plurality of types of solvents mixed in the second mixer 52 do not pass directly to the second separation column 54 as in the case of FIG. 3 but pass through the concentration column 63 and enter into the concentration column 63. After the concentrated sample is introduced, it is led to the second separation column 54.

  The sample thus introduced into the second separation column 54 is separated for each sample component in the process of passing through the second separation column 54, and is led to the cell 71 of the detector 7. Then, the measurement light from the light source 72 transmitted through the cell 71 is received by the light receiving unit 73, and the peak of each separated sample component is detected based on the received light intensity. As described above, the conventional analysis can be performed by analyzing the sample using the second separation column 54 using a plurality of types of solvents mixed in the second mixer 52 as a mobile phase.

  As described above, in the present embodiment, by rotating the first valve 55, the first communication state in which the first mixer 51 and the first separation column 53 communicate with the detector 7 (see FIGS. 1 and 2), Alternatively, the state is switched to the second communication state (see FIGS. 3 and 4) in which the second mixer 52 and the second separation column 54 communicate with the detector 7. That is, the first valve 55 constitutes a flow path switching unit for switching between the first communication state and the second communication state.

  In the present embodiment, it is possible to easily switch to the first communication state or the second communication state in which the internal capacity of the flow path is different simply by rotating the first valve 55 to switch. Therefore, the work for performing the analysis with different internal volumes is easy.

  In the present embodiment, the first mixer 51, the second mixer 52, the first separation column 53, and the second separation column 54 are all housed in the column oven 5. Therefore, the work of exchanging the mixers 51 and 52 and the work of exchanging the separation columns 53 and 54 can be performed at the same time, which further facilitates the work.

  In particular, in the present embodiment, since the flow path switching unit is configured by one valve (first valve 55), the internal capacity of the flow path differs only by switching this one valve (first valve 55). It is possible to easily switch to the first communication state or the second communication state. Thus, there is no need to synchronize the switching timing as in the case of switching a plurality of valves, so that the operation is further facilitated.

  Furthermore, in the present embodiment, the sample captured and concentrated in the concentration column 63 can be selectively guided to the first separation column 53 or the second separation column 54 only by rotating and switching the first valve 55. it can. Therefore, by easily switching to the first communication state or the second communication state in which the internal volume of the flow path is different, and guiding the concentrated sample to the first separation column 53 or the second separation column 54, any of the separation columns The analysis can be favorably performed using 53 and 54.

  The first mixer 51, the second mixer 52, the first separation column 53, the second separation column 54, the first valve 55, the second valve 64, the concentration column 63, and the like separate the sample components in the solvent to form a detector 7. Constitutes a flow path mechanism 100 for detection by means of. In the present embodiment, such a flow path mechanism 100 is configured to be housed in the column oven 5. Then, the sample component in the solvent separated by the first separation column 53 in the first communication state or the sample component in the solvent separated by the second separation column 54 in the second communication state is detected by the detector 7. Is done.

  Note that the first valve 55 and the second valve 64 are automatically switched under the control of a control unit (not shown) including a CPU. However, the configuration is not limited to such a configuration, and at least one of the first valve 55 and the second valve 64 may be manually switched.

  In the above embodiment, the case where the flow path switching unit for switching to the first communication state or the second communication state is configured by the first valve 55 has been described. However, the configuration is not limited to such a configuration, and the flow path switching unit may be configured by a valve other than the 10-port valve, or may be configured by a plurality of valves. Further, the flow path switching unit is not limited to the valve, and may be configured by another member.

  When the flow path switching unit is configured by a plurality of valves, for example, a flow path in which the first mixer 51 and the first separation column 53 communicate with each other, and a flow path in which the second mixer 52 and the second separation column 54 communicate with each other And a valve for selectively communicating the upstream side of these flow paths to the liquid feed pump 4 and a valve for selectively communicating the downstream side of these flow paths to the detector 7 are provided by a flow path switching unit. May be configured.

  The configuration other than the flow path mechanism is not limited to the configuration of the above embodiment, and any other configuration can be adopted. For example, the present invention is not limited to a configuration in which a single liquid pump 4 is used to perform a low-pressure gradient analysis, but may be applied to a configuration in which a plurality of liquid pumps are used to perform a high-pressure gradient analysis. It is.

DESCRIPTION OF SYMBOLS 1 Container 2 Deaeration unit 3 Low pressure gradient unit 4 Liquid feed pump 5 Column oven 6 Autosampler 7 Detector 51 First mixer 52 Second mixer 53 First separation column 54 Second separation column 55 First valve 56 Manifold 61 Needle 62 Syringe 63 Concentration column 64 Second valve 65 Sample introduction unit 71 Cell 72 Light source 73 Light receiving unit 100 Flow path mechanism

Claims (5)

A flow path mechanism for separating the sample components in the solvent and detecting with a detector,
A first mixer for mixing a solvent therein;
A second mixer having a capacity different from that of the first mixer and mixing a solvent therein;
A first separation column associated with the first mixer;
A second separation column associated with the second mixer;
Channel switching for switching to a first communication state in which the first mixer and the first separation column communicate with the detector, or a second communication state in which the second mixer and the second separation column communicate with the detector. Department and
The flow path mechanism, wherein the flow path switching unit is configured by one valve, and can be switched to the first communication state or the second communication state by simply switching the one valve.   The channel mechanism according to claim 1, further comprising a column oven that houses the first mixer, the second mixer, the first separation column, and the second separation column, and that is internally heated. In the one valve, a first port is connected to an inlet of the first mixer, a second port is connected to an outlet of the first mixer, and a third port is the second mixer. The fourth port is connected to the outlet of the second mixer, the fifth port is supplied with the solvent, and the sixth port is connected to the first separation column. , The seventh port is connected to the second separation column,
In the first communication state, the one valve is switched such that the fifth port communicates with the first port, and the second port communicates with the sixth port,
In the second communication state, the one valve is switched so that the fifth port communicates with the third port and the fourth port communicates with the seventh port. The flow path mechanism according to claim 1, wherein: Further comprising a concentration column for capturing and concentrating the sample,
In the first communication state, the sample concentrated in the concentration column is led to the first separation column,
The flow path mechanism according to any one of claims 1 to 3, wherein in the second communication state, the sample concentrated in the concentration column is led to the second separation column. A flow path mechanism according to any one of claims 1 to 4,
A detector for detecting a sample component in the solvent separated by the first separation column in the first communication state, or a sample component in the solvent separated by the second separation column in the second communication state. A liquid chromatograph comprising:

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