Extraction analysis system

Abstract

To shorten time required for analyzing a sample within a plurality of extraction containers held in a plurality of racks by overlapping a plurality of processes at a timing when the racks are replaced.SOLUTION: An extraction analysis device 2 is configured to set a plurality of extraction containers 10 held in a rack 8 placed on a placement table 12 as extraction targets in a preset order, to execute an extraction operation for extracting components from a sample to a mobile phase that is a supercritical fluid in the extraction container 10 set as the extraction target, and to execute analysis of the components by introducing the extracted components into an analysis channel 20. During the analysis of the components extracted from the sample by the extraction operation in the extraction container 10 set as a last extraction target among the plurality of extraction containers 10 held in the rack 8, the extraction analysis device 2 is configured to bring the rack 8 into a movable state in which the rack can be moved from the placement table 12, and a rack replacement device 4 is configured to execute replacement of the rack 8 on the placement table 12.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present invention relates to an extraction and analysis system that extracts a target component from a sample using a supercritical fluid and analyzes the extracted component. [Background technology]

[0002] Component extraction devices that extract components from samples using supercritical fluids are known. In such component extraction devices, extraction containers containing samples are held in a rack, and the rack is placed on a mounting table provided in the component extraction device. The rack can hold multiple extraction containers. Before component extraction, the sample in the extraction container is generally stored in a cooled state to prevent deterioration and volatilization. Meanwhile, before component extraction, the extraction container is heated to regulate the temperature of the extraction container in order to increase the component extraction efficiency.

[0003] Incidentally, a component extraction device has been proposed in which a heater or temperature sensor corresponding to each extraction container held in the rack is provided on the mounting table in order to individually control the temperature of the extraction containers held in a rack placed on the mounting table (see, for example, Patent Document 1). According to the proposed component extraction device, the temperature is controlled in each extraction container held in the rack immediately before component extraction is performed, thereby making it possible to standardize the temperature control time for the samples contained in each extraction container.

[0004] When performing online analysis of components extracted from samples in extraction vessels, the temperature control, extraction, and analysis processes must be repeated in sequence for each extraction vessel to perform the entire process from component extraction to analysis for all samples contained in the extraction vessels on a rack. For example, if a rack holds four extraction vessels and it takes 15 minutes to control the temperature, 10 minutes to extract, and 5 minutes to analyze, it will take 30 minutes for each extraction vessel, meaning it will take at least two hours to complete the analysis of the samples in all extraction vessels on the rack.

[0005] Furthermore, by adjusting the temperature of the next extraction vessel while extracting components or analyzing the extracted components in one extraction vessel, the time required to complete the analysis of samples in all extraction vessels held in the rack can be shortened. [Prior art documents] [Patent documents]

[0006] [Patent Document 1] Japanese Patent Application Publication No. 2017-146127 Summary of the Invention [Problem to be solved by the invention]

[0007] Because there is a limit to the number of extraction vessels that can be held on a single rack, when there are many samples to be analyzed, it is necessary to hold multiple extraction vessels on multiple racks and sequentially exchange the racks on the loading platform of the component extraction device. The exchange of racks on the loading platform can be performed automatically by a rack exchanger. In previous systems equipped with a rack exchanger, when analysis of samples in extraction vessels held on a rack on the loading platform was completed, the management device managing the system notified the rack exchanger that processing of all extraction vessels on the rack on the loading platform was completed, and the rack exchanger then exchanged the rack on the loading platform. Therefore, when rack exchange was required, multiple processes could not be performed overlappingly, and there was a limit to shortening the time required to complete a series of processes for a large number of samples that required the use of multiple racks.

[0008] The present invention has been made in consideration of the above-mentioned problems, and aims to shorten the time required to analyze samples in multiple extraction containers held in multiple racks by overlapping multiple processes at times when racks are replaced. [Means for solving the problem]

[0009] The extraction analysis system according to the present invention is an extraction analysis system including an extraction analysis device and a rack exchange device, The extraction analysis device has a mounting table for mounting a rack holding a plurality of extraction containers, and an analysis flow path for analyzing components extracted from a sample, and is configured to select the plurality of extraction containers held in the rack mounted on the mounting table as extraction targets in a predetermined order, perform an extraction operation to extract components from the sample into a mobile phase, which is a supercritical fluid, in the extraction target extraction container, and introduce the components extracted in the extraction operation into the analysis flow path to analyze the components in the analysis flow path. the rack exchange device is configured to exchange the rack on the table by moving the rack from the table of the extraction analysis device and placing the rack on the table; the extraction analysis device is configured to be in a movable state in which the rack can be moved from the mounting table during the analysis of the components extracted from the sample by the extraction operation in the extraction container that is the last extraction target among the plurality of extraction containers held in the rack, The rack exchange device is configured to exchange the rack on the mounting table during the analysis of the components extracted by the extraction operation in the extraction container that is the final extraction target. [Effects of the Invention]

[0010] According to the extraction analysis system of the present invention, the extraction analysis device makes the rack movable so that it can be moved from the mounting base during the analysis of the components extracted from the sample by the extraction operation in the extraction container that is the last extraction target among the multiple extraction containers held in the rack, and the rack exchange device exchanges the rack on the mounting base during the analysis of the components extracted by the extraction operation in the extraction container that is the last extraction target.Therefore, it is possible to overlap the rack exchange and the processing after the rack exchange at the time of rack exchange, and the time required to analyze the samples in the multiple extraction containers held in the multiple racks is shortened. [Brief explanation of the drawings]

[0011] [Figure 1] 1 is a schematic diagram illustrating an example of an extraction and analysis system. [Figure 2] FIG. 10 is a diagram showing the flow path configuration during extraction of components from a sample in the same example. [Figure 3] FIG. 10 is a diagram showing the flow path configuration when components extracted in an extraction container are introduced into an analysis flow path in this example. [Figure 4] FIG. 2 is a diagram showing the flow path configuration in the analysis mode in the same embodiment. [Figure 5] 10 is a timing chart showing an example of the execution timing of a series of processes for samples in a plurality of extraction containers held in a plurality of racks in the same embodiment. DETAILED DESCRIPTION OF THE INVENTION

[0012] Hereinafter, an embodiment of an extraction analysis system according to the present invention will be described with reference to the drawings.

[0013] FIG. 1 shows an example of an extraction and analysis system.

[0014] The extraction analysis system 1 of this embodiment includes an extraction analysis device 2, a rack exchange device 4, and a controller 6.

[0015] The extraction analysis device 2 mainly includes a mounting table 12, a mobile phase supply unit 14, an extraction valve 16, a vent valve 18, an analysis flow path 20, a needle 36, and a back pressure control valve (hereinafter, referred to as BPR) 46.

[0016] A rack 8 is placed on the mounting base 12. The rack 8 can hold multiple (four in this embodiment) extraction vessels 10. Each extraction vessel 10 has an internal space for accommodating a sample and extracting components from the sample, and is provided with ports on both the top and bottom surfaces that lead to the internal space. The mounting base 12 is provided with connecting pipes 22 and heaters 24 at positions corresponding to each of the extraction vessels 10 held in the rack 8 to be placed. The connecting pipes 22 are thin tubes that are inserted into ports on the bottom surfaces of the extraction vessels 10 held in the rack 8 when the rack 8 is placed in a predetermined position on the mounting base 12, thereby fluidly connecting them to the internal spaces of the extraction vessels 10. The heaters 24 are in contact with the bottom surfaces of the extraction vessels 10 held in the rack 8 when the rack 8 is placed in a predetermined position on the mounting base 12, thereby individually heating each of the extraction vessels 10.

[0017] Mobile phase supply 14 supplies liquid carbon dioxide and modifier via pumps 30 and 32. The liquid carbon dioxide and modifier are mixed in mixer 34. Mobile phase supply 14 is fluidly connected to a central common port of extraction valve 18, which will be described below.

[0018] The extraction valve 16 has a common port located in the center and selective ports numbered 1 to 6 located around the common port, and is configured to fluidically connect the common port to any one of the selective ports numbered 1 to 6. As described above, the mobile phase supply unit 14 is fluidly connected to the common port of the extraction valve 16. Each of the selective ports numbered 1 to 4 of the extraction valve 16 is fluidly connected to a flow path leading to the connecting pipe 22 of the mounting table 12. By fluidly connecting the common port of the extraction valve 16 to the selective ports numbered 1 to 4, the mobile phase from the mobile phase supply unit 14 can be supplied to the desired extraction container 10 of the rack 8 mounted on the mounting table 12. The home port 52, which serves as the home position of the needle 36 described below, is fluidly connected to the home port 52 of the vent valve 18 described below. The home port 52 of the extraction valve 16 is fluidly connected to the home port 52 of the vent valve 18 described below.

[0019] Vent valve 18 is a two-position valve that has ports numbered 1 to 6 arranged on the same circumference and fluidly communicates between adjacent ports. That is, vent valve 18 can be placed in either a first state (state in FIG. 1) in which ports 1 and 6, ports 2 and 3, and ports 4 and 5 are fluidly communicated, or a second state (state in FIG. 4) in which ports 1 and 2, ports 3 and 4, and ports 5 and 6 are fluidly communicated.

[0020] As mentioned above, port 5 of vent valve 18 is fluidly connected to port 6 of extraction valve 16, and ports 4 and 6 adjacent to port 6 are fluidly connected to extraction channel 38 and analysis channel 20, respectively, which lead to needle 36. Port 1 of vent valve 18 is fluidly connected to branch channel 42 branching from extraction channel 38 via T-shaped piping 40, and ports 2 and 3 each lead to a drain.

[0021] The analytical flow path 20 is equipped with a separation column 48 and a detector 50. The BPR 46 is provided on the analytical flow path 20 and serves to control the pressure in the system from the mobile phase supply unit 14 to the analytical flow path 20 so that the mobile phase supplied from the mobile phase supply unit 14 becomes a supercritical fluid. In this embodiment, the BPR 46 is provided after the detector 50, but the position of the BPR 46 on the analytical flow path 20 can be changed.

[0022] The needle 36 can be moved horizontally and vertically by a movement mechanism (not shown). The needle 36 is inserted tip-first into a port on the top surface of the extraction vessel 10 held in the rack 8 placed on the mounting table 12, thereby fluidly connecting the extraction channel 38 with the extraction vessel 10.

[0023] The extraction analysis device 2 further includes a washing port 54. A washing solution is supplied to the washing port 54 by a pump 56, and the needle 36 can be washed as needed.

[0024] Although not shown in detail in the figure, the rack exchange device 4 comprises a storage cabinet that stores a plurality of racks 8 and an arm that moves between the storage cabinet and the mounting table 12 of the extraction analysis device 2, and is a device that places racks 8 on the mounting table 12 of the extraction analysis device 2 and moves racks 8 from the mounting table 12, thereby exchanging racks 8 on the mounting table 12. Racks 8 stored in the storage cabinet are assigned rack numbers that indicate their storage positions within the storage cabinet as rack information.

[0025] The controller 6 manages the operation of the extraction / analysis system 1 by issuing operational instructions to the extraction / analysis apparatus 2 and the rack exchanger 4 according to a preset operational sequence. In this embodiment, the operational sequence is set by an analysis batch, in which the operations and conditions to be executed by the extraction / analysis apparatus 2 and the rack exchanger 4 are written in each batch line. The controller 6 sequentially reads the batch lines written in the analysis batch and issues operational instructions to the extraction / analysis apparatus 2 and / or the rack exchanger 4 according to the operational conditions written in each batch line, thereby operating the extraction / analysis apparatus 2 and / or the rack exchanger 4. For example, when replacing the rack 8 on the mounting table 12 of the extraction / analysis apparatus 2, the controller 6 reads the rack number written in the corresponding batch line of the analysis batch and provides information to the rack exchanger 4 regarding the location of the rack 8 stored in the storage room to replace the rack 8 on the mounting table 12 with. The controller 6 can be implemented by a dedicated computer or a general-purpose personal computer.

[0026] Here, each process in the extraction analysis device 2 will be described with reference to FIGS.

[0027] First, the extraction container 10 containing the sample to be analyzed is heated to a predetermined temperature. The temperature of the extraction container 10 is adjusted immediately before the component extraction process described below is performed. Therefore, at this stage, the temperature of the extraction container 10 that is not the extraction target is not adjusted.

[0028] After the temperature adjustment of the extraction vessel 10 is completed as described above, as shown in FIG. 2, a needle 36 is inserted into the extraction vessel 10 to be extracted, the common port of the extraction valve 16 is fluidly connected to port 6, and the vent valve 18 is set to its first position to fluidly connect ports 4 and 5. The mobile phase from the mobile phase supply unit 14 is supplied to the extraction vessel 10 to be extracted through the extraction flow path 38, and the mobile phase is filled into the extraction vessel 10 to be extracted. At this time, the system from the mobile phase supply unit 14 to the extraction vessel 10 is controlled to a predetermined pressure by the BPR 46, and the mobile phase that has become a supercritical fluid is filled into the extraction vessel 10. This state is maintained until a predetermined time has elapsed since the mobile phase was filled into the extraction vessel 10 to be extracted, and the sample components are extracted into the mobile phase in the extraction vessel 10.

[0029] After the above extraction process is completed, as shown in Figure 3, the extraction valve 16 is switched so that the mobile phase supply unit 14 is fluidly connected to the extraction vessel 10 of the extraction target, and the mobile phase is fed from the mobile phase supply unit 14. By supplying the mobile phase from below the extraction vessel 10 of the extraction target, the mobile phase containing the components extracted from the sample in the extraction vessel 10 is introduced into the analysis channel 20 via the extraction channel 38, the T-shaped pipe 40, the branch channel 42, and the vent valve 18.

[0030] After the components are introduced into the analytical flow path 20, as shown in Figure 4, the extraction valve 16 is switched to a second state so that the common port and port 6 are fluidly connected, and the vent valve 18 is switched to a second state so that ports 5 and 6 are fluidly connected, so that the mobile phase supply unit 14 is fluidly connected to the analytical flow path 20 without passing through the extraction flow path 38 and the branch flow path 42. This state is called the analytical mode. In this analytical mode, the mobile phase is supplied from the mobile phase supply unit 14 to the analytical flow path 20, and the components introduced into the analytical flow path 20 are guided to a separation column for separation and then detected by the detector 50.

[0031] The extraction analysis device 2 selects the extraction containers 10 on the rack 8 placed on the mounting table 12 as extraction targets in a preset order, and sequentially performs the above-described processes from temperature control to analysis on the extraction containers 10 that have been selected as extraction targets. The extraction analysis device 2 outputs a replaceable signal to the controller 6 when the components extracted from the sample in the extraction container 10 that was last selected as an extraction target among the extraction containers 10 on the rack 8 placed on the mounting table 12 are introduced into the analysis flow path 20 and the device transitions to the analysis mode shown in Figure 4.

[0032] In the analysis mode of FIG. 4 , both the extraction vessel 10 and the needle 36 that were the extraction targets are disconnected from the mobile phase supply unit 14 and the analysis flow path 20, so the needle 36 can be withdrawn from the extraction vessel 10. After the needle 36 is withdrawn from the extraction vessel 10, the rack 8 is placed in a movable state in which it can be moved from the mounting base 12. At this time, analysis of the components extracted in the extraction vessel 10 that was the last extraction target is being performed, but the rack 8 on the mounting base 12 is replaceable. Upon receiving a replacement enable signal from the extraction / analysis apparatus 2, the controller 6 reads the next batch line of the analysis batch and sends information about a new rack 8 to be placed on the mounting base 12 together with a rack replacement signal to the rack replacement device 4. Upon receiving the rack replacement signal from the controller 6, the rack replacement device 4 replaces the rack 8 on the mounting base 12 with a new rack 8 in accordance with the information received along with the rack replacement signal.

[0033] In typical batch processing, the next batch line is read and processed when the processing of the currently running batch line is completed. That is, when typical batch processing is applied to this extraction analysis system, the controller 6 reads the next batch line of the analysis batch when the controller 6 receives a completion signal from the extraction analysis apparatus 2 indicating that the analysis of the components extracted from the sample in the extraction container 10 in the extraction analysis apparatus 2 is complete. Therefore, even if the component being analyzed was extracted from the last extraction container 10 in the rack 8 on the mounting table 12, the rack 8 on the mounting table 12 will not be replaced before the analysis is completed. In contrast, in this embodiment, the controller 6 reads the next batch line when it receives a replacement enable signal from the extraction analysis apparatus 2, so that the rack 8 can be replaced while the analysis of the component extracted from the last extraction container 10 is being performed.

[0034] Furthermore, when the rack 8 on the mounting table 12 is replaced with a new one, the controller 6 receives a replacement completion signal from the rack replacement device 4, reads the next batch line, and causes the extraction analysis device 2 to start temperature control of the extraction container 10 of the next extraction target. In this way, in this embodiment, by replacing the rack 8 on the mounting table 12 and starting temperature control of the extraction container 10 of the next extraction target while analysis of the components extracted in the extraction container 10 of the previous extraction target is being performed, the time required for a series of processes of samples in multiple extraction containers 10 held in multiple racks 8 can be shortened.

[0035] FIG. 5 is a timing chart for explaining an example of the execution timing of a series of processes for samples in a plurality of extraction containers 10 held in a plurality of racks 8.

[0036] As shown in FIG. 5, for each extraction container 10 (container 1 to container 4) held in the same rack 8, temperature control, component extraction (extraction), introduction of the extracted components into the analysis flow path 20 (introduction), and analysis are sequentially performed. In this embodiment, temperature control of the extraction container 10 of the next extraction target is started while processes such as extraction, introduction, and analysis are being performed on the sample in the extraction container 10 of the previous extraction target. This shortens the time required to complete analysis of all samples in the multiple extraction containers 10 held in multiple racks 8 compared to starting temperature control of the extraction container 10 of the next extraction target after analysis of the components extracted in the extraction container 10 of the previous extraction target is completed. Note that the timing for starting temperature control of the extraction container 10 of the next extraction target can be determined taking into account the respective times required for temperature control, extraction, introduction, and analysis, so that the extraction analysis device 2 can immediately perform the extraction process when the extraction analysis device 2 is ready to perform the component extraction process in the extraction container 10 of the next extraction target.

[0037] 5, immediately after analysis of the components extracted in the last extraction container 10 (container 4 in rack 1) is started, the rack exchange device 4 exchanges rack 8 from rack 1 to rack 2, and while the analysis is in progress, temperature control of the first extraction container 10 (container 1) in the new rack 8 (rack 2) is started. This makes it possible to overlap the processing of the sample in the previous extraction container 10 and the processing of the sample in the next extraction container 10, even when the rack 8 is exchanged, further reducing the time required to complete the analysis of the samples in the multiple extraction containers 10 held in multiple racks 8.

[0038] Generally, when the analysis of all samples in the extraction containers 10 on the racks set in the extraction analyzer is completed, the extraction analyzer outputs a completion signal, but the rack exchanger cannot know when to exchange the rack until the completion signal is output from the extraction analyzer. In contrast, in this embodiment, the extraction analyzer 2 outputs an exchangeable signal when the rack 8 becomes exchangeable, so that the rack exchanger 4 can exchange the rack 8 before the analysis of all samples in all the extraction containers 10 on the racks 8 set in the apparatus is completed, allowing overlapping of processing at the time when the rack 8 is exchanged.

[0039] The embodiment described above is merely one example of an embodiment of the extraction and analysis system according to the present invention. The embodiment of the extraction and analysis system according to the present invention is as follows.

[0040] One embodiment of the extraction analysis system according to the present invention is an extraction analysis system including an extraction analysis device and a rack exchange device, The extraction analysis device has a mounting table for mounting a rack holding a plurality of extraction containers, and an analysis flow path for analyzing components extracted from a sample, and is configured to select the plurality of extraction containers held in the rack mounted on the mounting table as extraction targets in a predetermined order, perform an extraction operation to extract components from the sample into a mobile phase, which is a supercritical fluid, in the extraction target extraction container, and introduce the components extracted in the extraction operation into the analysis flow path to analyze the components in the analysis flow path. the rack exchange device is configured to exchange the rack on the table by moving the rack from the table of the extraction analysis device and placing the rack on the table; the extraction analysis device is configured to be in a movable state in which the rack can be moved from the mounting table during the analysis of the components extracted from the sample by the extraction operation in the extraction container that is the last extraction target among the plurality of extraction containers held in the rack, The rack exchange device is configured to exchange the rack on the mounting table during the analysis of the components extracted by the extraction operation in the extraction container that is the final extraction target.

[0041] In the aspect [1] of the above embodiment, the extraction analysis device is configured to include a heater on the mounting table for individually heating each of the extraction containers held in the rack, and to perform a temperature control operation using the heater to adjust the temperature of the extraction container to a set temperature before performing the extraction operation in the extraction container selected as the extraction target, The extraction analysis device is configured to start the temperature control operation on the extraction container that is the first extraction target among the multiple extraction containers held in the rack newly placed on the mounting table after the rack on the mounting table has been replaced by the rack replacement device and before the analysis in the analysis flow path is completed.

[0042] In aspect [2] of the above embodiment, the extraction analysis device outputs a rack exchangeable signal immediately after the rack becomes movable, The rack exchange device is configured to execute the exchange of the rack due to the rack exchangeable signal output from the extraction analysis device. This aspect [2] can be combined with the above aspect [1].

[0043] In the above aspect [2], a controller may be provided that controls the operation of the extraction analysis device and the rack exchange device using a preset operation sequence for the rack set in the rack exchange device, The controller can be configured to obtain rack information regarding the rack to be next placed on the table from the operation sequence when it receives the rack exchangeable signal output from the extraction analysis device, and notify the rack exchange device of the obtained rack information.

[0044] Furthermore, the controller can receive the rack exchangeable signal from the extraction and analysis device during the analysis of the components extracted by the extraction operation in the extraction vessel that is the last extraction target. [Explanation of symbols]

[0045] 1 Extraction and Analysis System 2 Extraction analysis device 4 Rack exchange device 6 Controller 8 racks 10 Extraction vessel 12 Mounting table 14 Mobile phase supply section 16 Extraction valve 18 Vent valve 20 Analysis channel 22 Connecting pipe 24 Heater 30, 32, 56 Pump 34 Mixer 36 Needle 38 Extraction channel 40 T-pipe 42 Branch channel 46 Back Pressure Control Valve (BPR) 48 Separation Column 50 detectors 52 Home Port 54 Washing port

Claims

1. An extraction analysis system including an extraction analysis device and a rack exchange device, The extraction analysis device has a mounting table for mounting a rack holding a plurality of extraction containers, and an analysis flow path for analyzing components extracted from a sample, and is configured to select the plurality of extraction containers held in the rack mounted on the mounting table in a preset order as extraction targets, perform an extraction operation for extracting components from the sample into a mobile phase, which is a supercritical fluid, in the extraction container selected as the extraction target, and introduce the components extracted in the extraction operation into the analysis flow path to analyze the components in the analysis flow path. the rack exchange device is configured to perform exchange of the rack on the mounting table by moving the rack from the mounting table of the extraction analysis device and placing the rack on the mounting table, the extraction analysis device is configured to be in a movable state in which the rack can be moved from the placement table during the analysis of the components extracted from the sample by the extraction operation in the extraction container that is the last extraction target among the plurality of extraction containers held in the rack, An extraction and analysis system, wherein the rack exchange device is configured to perform exchange of the rack on the placement table during the analysis of the components extracted by the extraction operation in the extraction container that is the final extraction target.

2. The extraction analysis device is configured to include a heater on the mounting table for individually heating each of the extraction containers held on the rack, and to perform a temperature control operation using the heater to adjust the temperature of the extraction container to a set temperature before performing the extraction operation in the extraction container that is the extraction target, 2. The extraction analysis system according to claim 1, wherein the extraction analysis device is configured to start the temperature control operation on the extraction vessel that is the first extraction target among the plurality of extraction vessels held in the rack newly placed on the mounting table after the rack on the mounting table is replaced by the rack replacement device and before analysis in the analysis flow path is completed.

3. the extraction and analysis device outputs a rack exchangeable signal immediately after the rack becomes movable; The extraction analysis system of claim 1 , wherein the rack exchanger is configured to execute the exchange of the rack due to the rack exchangeable signal output from the extraction analysis device.

4. a controller for controlling operations of the extraction analysis device and the rack exchange device using a preset operation sequence for the rack set in the rack exchange device; The extraction and analysis system according to claim 3, wherein the controller is configured to obtain rack information regarding the rack to be next placed on the mounting table from the operation sequence when the controller receives the rack exchangeable signal output from the extraction and analysis device, and to notify the rack exchange device of the obtained rack information.

5. The extraction and analysis system of claim 4, wherein the controller is configured to receive the rack exchangeable signal from the extraction and analysis device during the analysis of the components extracted by the extraction operation in the extraction vessel that is the last extraction target.

Images