WO2024095765A1 - 液体クロマトグラフの制御方法および液体クロマトグラフ - Google Patents

液体クロマトグラフの制御方法および液体クロマトグラフ Download PDF

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Publication number
WO2024095765A1
WO2024095765A1 PCT/JP2023/037573 JP2023037573W WO2024095765A1 WO 2024095765 A1 WO2024095765 A1 WO 2024095765A1 JP 2023037573 W JP2023037573 W JP 2023037573W WO 2024095765 A1 WO2024095765 A1 WO 2024095765A1
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Prior art keywords
separation column
liquid chromatograph
liquid delivery
liquid
delivery device
Prior art date
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Ceased
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PCT/JP2023/037573
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English (en)
French (fr)
Japanese (ja)
Inventor
和彦 坂本
拓実 山田
直人 坂本
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Hitachi High Tech Corp
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Hitachi High Tech Corp
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Priority to JP2024554382A priority Critical patent/JPWO2024095765A1/ja
Priority to EP23885527.4A priority patent/EP4614141A1/en
Priority to CN202380072099.3A priority patent/CN120019274A/zh
Publication of WO2024095765A1 publication Critical patent/WO2024095765A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/38—Flow patterns
    • G01N30/46—Flow patterns using more than one column
    • G01N30/466—Flow patterns using more than one column with separation columns in parallel
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/16—Injection
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature

Definitions

  • the present invention relates to a method for controlling a liquid chromatograph and a liquid chromatograph.
  • a liquid chromatograph is an analytical device that identifies components by utilizing the property that when a mixed sample solution containing the components to be measured is injected into a separation column through which a solvent is continuously delivered by a delivery pump, the components in the sample interact with the packing material and solvent of the separation column according to their chemical properties, and are detected at different times depending on the differences in the interactions between the components.
  • Detectors used in liquid chromatographs include photometers and mass spectrometers, which are appropriately selected depending on the analytical purpose and materials.
  • Liquid chromatographs that connect multiple separation columns in parallel to a liquid delivery pump are also known (Patent Document 1).
  • a step of using a liquid delivery device in a process of replacing a separation column, among the steps after connecting the separation column to a flow path, a step of using a liquid delivery device is carried out so as not to overlap with a process using a flow path that is not the subject of the separation column replacement.
  • the present invention makes it easier to avoid conflicts between the separation column replacement process and scheduled analysis operations.
  • FIG. 1 shows the configuration of a liquid chromatograph according to the present embodiment.
  • 4 is a flowchart showing a method for controlling a liquid chromatograph according to the present embodiment.
  • Schedule for each separation column in this embodiment Schedule for each separation column in this embodiment.
  • Schedule for each separation column in this embodiment Schedule for each separation column in this embodiment.
  • Schedule for each separation column in this embodiment. 1 shows an example of a separation column replacement process according to the present embodiment.
  • Fig. 1 shows the configuration of a liquid chromatograph according to this embodiment.
  • the liquid chromatograph includes flow paths 104 and 106 to 110.
  • a plurality of separation columns 105 (five in the example of Fig. 1) are arranged in the five flow paths, and in particular, separation column 105a is arranged in flow path 106, separation column 105b is arranged in flow path 107, separation column 105c is arranged in flow path 108, separation column 105d is arranged in flow path 109, and separation column 105e is arranged in flow path 110.
  • No separation column 105 is arranged in flow path 104.
  • each flow path is connected to flow path switching valve 103, and the end of each flow path is connected to flow path switching valve 111.
  • Flow path switching valves 103 and 111 are connected to flow path switching valve 114.
  • detector 112 liquid delivery device 101 (e.g., a pump), and liquid delivery device 113 (e.g., a pump) are connected to flow path switching valve 114.
  • Liquid delivery devices 101 and 113 can each deliver a different solvent 115 (which may be a solution containing a solute such as a reagent) via flow path switching valve 114.
  • the flow path switching valve 114 and the liquid delivery device 101 are connected via the sample injection section 102, and it is possible to inject a sample (i.e., a specimen to be tested) from the sample injection section 102 into the solvent delivered from the liquid delivery device 101.
  • the liquid delivery device 113 delivers a solvent (cleaning solution, etc.) that does not require the injection of a sample.
  • the liquid delivery devices 101 and 113 inject a mixed sample solution containing the components to be measured into the separation column 105.
  • Different contents fillers and/or solvents
  • Each component in the sample interacts with a different content of the separation column 105 according to its chemical properties, and is configured to reach the detector 112 at different times according to differences in the interactions between the components. In this way, the components to be measured can be detected and/or measured.
  • the detector 112 is, for example, a photometer, a mass spectrometer, etc.
  • the liquid chromatograph has multiple flow paths 106-110 that share the liquid delivery devices 101 and 113, and each of these flow paths is provided with a separation column 105.
  • a control device may be provided to control the operation of the liquid chromatograph.
  • the control device may execute the liquid chromatograph control method described herein, thereby controlling the operation of the liquid chromatograph.
  • the configuration of the liquid chromatograph is not limited to that shown in FIG. 1, and the analytical operation of the liquid chromatograph is not limited to that described above.
  • Those skilled in the art can appropriately design or modify the configuration and operation of the liquid chromatograph based on publicly known techniques, etc.
  • FIG. 7 shows an example of a separation column replacement process according to this embodiment.
  • separation column is simply written as “column.”
  • the liquid chromatograph allows analysis operations to continue in parallel in the flow paths that are not targeted for replacement of the separation column 105, in order to avoid a situation in which the entire rapid LC stream becomes unusable.
  • a liquid chromatograph performs analysis operations on flow paths that are not the target of separation column replacement in parallel with separation column replacement.
  • the separation column replacement process requires the use of liquid delivery devices 101 and 113, and these liquid delivery devices are also used in the analysis operations.
  • a set of liquid delivery devices (liquid delivery device 101 and liquid delivery device 113) is shared by multiple (e.g., five) flow paths, so if an attempt is made to perform analysis operations on flow paths that are not the target of separation column replacement in parallel with the entire separation column replacement process, contention for the liquid delivery devices will occur.
  • the liquid chromatograph is controlled so that, in the process of replacing a separation column, among the steps after connecting the separation column to the flow path, the steps that do not use the liquid delivery device are performed in parallel with processes (e.g., analytical operations) that use flow paths that are not the subject of separation column replacement, and the steps that use the liquid delivery device are performed so as not to overlap with processes that use flow paths that are not the subject of separation column replacement.
  • processes e.g., analytical operations
  • the only separation column replacement process that uses a liquid delivery device is the major step "Preparation after separation column replacement.” More specifically, within the major step “Preparation after separation column replacement,” the sub-step “Liquid delivery” uses a liquid delivery device, while the sub-steps “Start of post-replacement preparation” and “Completion of post-replacement preparation” do not use a liquid delivery device. The major step “Preparation before separation column replacement” and the major step “Separation column replacement operation” do not use a liquid delivery device.
  • the liquid chromatograph can carry out processes that do not use a liquid delivery device and analytical operations in flow paths that are not subject to separation column replacement in parallel.
  • the liquid chromatograph also schedules the process that uses the liquid delivery device to the nearest free cycle at the time of scheduling (for example, a cycle that does not overlap with a process that uses a flow path that is not the subject of separation column replacement).
  • FIG. 2 is a flowchart showing a method for controlling a liquid chromatograph according to this embodiment.
  • FIGS. 3 to 6 show schedules at various times for each separation column in this embodiment. Schedules are created for the five separation columns 105a to 105e and the liquid delivery devices 101 and 113.
  • the operation in FIG. 2 is started in response to the occurrence of a request to replace a separation column. For example, assume that a replacement request 302 is made for separation column 105a at current time 305 in FIG. 3. First, the liquid chromatograph searches for and identifies the flow path that is the subject of the replacement request (step 201).
  • a process that uses separation column 105a (e.g., an analytical operation in separation column 105a) is identified as a process that uses flow path 106, which is the target of separation column replacement.
  • a process that uses any of separation columns 105b-105e (e.g., an analytical operation in any of separation columns 105b-105e) is identified as a process that uses any of flow paths 107-110, which are not the target of separation column replacement.
  • the liquid chromatograph searches for and identifies the scheduled cycle (the last one, if there are multiple) in the separation column 105a (step 202). In the example of FIG. 3, the cycle of the analysis operation 303 is scheduled.
  • the liquid chromatograph temporarily suspends the scheduling of analytical operations after the scheduled cycle (step 203). That is, in the separation column 105a, the scheduling of a new analytical operation after the analytical operation 303 is temporarily prohibited. Note that in FIG. 3, for separation columns 105b to 105e indicated with an "O" as the schedulability 301, it remains possible to schedule a new analytical operation, whereas for separation column 105a indicated with an "X", the scheduling of a new analytical operation is prohibited.
  • step 204 determines whether the scheduling of the analysis operation after the scheduled cycle has been paused. In other words, it determines whether the processing of step 203 has been executed. If it has not been paused, step 204 is executed repeatedly.
  • the liquid chromatograph executes a pre-exchange preparation process for the separation column 105a (step 205).
  • a pre-exchange preparation process for the separation column 105a As shown in FIG. 4, when the last analysis operation already scheduled for the separation column 105a (the one searched for in step 202, for example, analysis operation 303 in FIG. 3) is completed, the pre-exchange preparation process for the column 105a 402 and the column exchange operation 403 are scheduled and executed over time.
  • the column replacement preparation 402 and the column replacement operation 403 are performed in parallel with the analysis operation using the flow paths 107-110 that are not the subject of separation column replacement (naturally, it is also possible to perform them so as not to overlap with the analysis operation).
  • analysis operations and scheduling of analysis operations can continue to be performed in the flow paths 107-110 (associated with separation columns 105b-105e) that are not the subject of separation column replacement.
  • a new analysis operation for example, analysis operation 404 in separation column 105b is scheduled.
  • the liquid chromatograph determines whether the preparatory process before the separation column replacement is complete (step 206), and if not, repeats step 206.
  • the liquid chromatograph executes the separation column replacement operation (step 207). This replaces the separation column 105a.
  • the liquid chromatograph checks whether the separation column replacement operation is complete (step 208). If it is not complete, the liquid chromatograph may wait until the operation is complete without terminating step 208.
  • the liquid chromatograph searches for and identifies the last scheduled analytical operation for all flow paths (step 209).
  • the last scheduled analytical operation is analytical operation 404.
  • the liquid chromatograph schedules a post-separation column replacement preparation process after the analysis operation 404 identified in step 209 (step 210). For example, as shown in FIG. 5, a future post-separation column replacement preparation 504 is scheduled at the current time 506.
  • the post-separation column replacement preparation 504 occupies the liquid delivery device 101 or 113.
  • post-separation column replacement preparation 504 is scheduled for the liquid delivery device, which occupies the liquid delivery device, analysis operations cannot be scheduled for separation column 105a or the other separation columns 105b to 105e during the cycle in which post-separation column replacement preparation 504 is performed. For cycles after post-separation column replacement preparation 504 is completed, analysis operations can be scheduled (for example, analysis operation 505 in FIG. 5).
  • the liquid chromatograph executes post-exchange preparation processing (step 211).
  • this step 211 is executed after the separation column is replaced (i.e., after step 208).
  • the post-exchange preparation processing is the process after the column replacement operation 403 (i.e., the process after the new separation column is connected to the flow path).
  • the start step of the post-replacement preparation process for the separation column includes a step of determining whether or not there is a sufficient amount of system reagent remaining.
  • the remaining amount of system reagent can be detected, for example, using a remaining amount detection device provided on the container.
  • whether or not there is a sufficient amount of system reagent remaining can be determined, for example, by comparing it with the amount of system reagent required for the subsequent substep "liquid delivery".
  • the process proceeds to the subsequent step 212. If there is an insufficient amount of system reagent remaining, the preparation process after the separation column replacement may not be able to be executed, so a warning message indicating that there is an insufficient amount of system reagent remaining may be output to prompt the user to take action.
  • the liquid chromatograph may recognize the type of separation column that will be newly installed by replacing the separation column, and may determine the liquid delivery conditions for the system reagent according to the recognized type.
  • the contents of the liquid delivery conditions can be defined appropriately by those skilled in the art, but may include, for example, flow rate, liquid delivery time, etc.
  • the liquid chromatograph delivers the system reagent based on the determined liquid delivery conditions, and delivers the system reagent to the newly installed separation column. This type of control allows processing to be performed under appropriate conditions according to various types of separation columns.
  • the system reagent delivery conditions may be defined as multiple patterns. In that case, when determining the system reagent delivery conditions, one of the multiple patterns is selected according to the type of separation column to be newly installed, and the delivery conditions are determined. In this way, when there are many types of separation columns, there is no need to define individual delivery conditions for all of the separation columns, and delivery conditions can be set efficiently.
  • liquid delivery process of the preparation process after replacing the separation column may include a step of controlling the temperature of the new separation column until it reaches a predetermined temperature.
  • the liquid delivery process of the preparation process after the separation column replacement may include a process of determining whether or not to perform temperature control of the separation column, and a process of selecting temperature control parameters if temperature control of the separation column is to be performed.
  • the liquid chromatograph may determine whether or not to perform temperature control of the separation column depending on the type of the newly installed separation column. Also, if temperature control of the separation column is to be performed, temperature control parameters may be selected depending on the type of the newly installed separation column.
  • the next analytical operation is performed at a more appropriate temperature, improving analytical accuracy and/or efficiency.
  • step 212 the liquid chromatograph determines whether the post-separation column replacement preparation process has been completed (step 212), and if not, repeats step 212. At this point, the current time becomes current time 606 in FIG. 6(a). When the post-separation column replacement preparation process has been completed, the liquid chromatograph ends the process in FIG. 2.
  • the temporary suspension process (prohibition of scheduling a new analysis operation) that occurred in step 203 is released when the process in FIG. 2 ends.
  • schedulability 601 for separation column 105a changes from "x" to "o”
  • a new analysis operation can be scheduled for separation column 105a.
  • analysis operation 611 is a process that follows column replacement operation 403 (i.e., a process that follows connecting a new separation column to the flow path).
  • analytical operations using the flow paths 107-110 (associated with separation columns 105b-105e) that are not the subject of separation column replacement can be performed either before or after the post-separation column replacement preparation process.
  • a process using the flow path 106 (associated with separation column 105a) that is the subject of separation column replacement cannot be performed before the post-separation column replacement preparation process, and is performed after post-separation column replacement preparation 504, such as analytical operation 611. In this way, it is possible to prevent analytical operations from being scheduled for flow paths that are undergoing separation column replacement.
  • liquid chromatograph control method and liquid chromatograph of this embodiment it is possible to replace the separation column without stopping the analysis operations of the entire rapid LC stream and the scheduling of the analysis operations. In other words, it is possible to more easily avoid conflicts between the separation column replacement process and scheduled analysis operations.
  • the liquid chromatography section has two types of streams, HPLC and Rapid LC, and since the configurations used for each are different, it is necessary to schedule the separation column replacement appropriately for each.
  • HPLC a method (addition method) is used in which separation column replacement is scheduled after the last analysis operation that has already been scheduled.
  • separation column replacement at the user's discretion can be requested at any time, regardless of the expiration date or remaining number of uses of the target separation column. Therefore, when a request for separation column replacement is made, an analysis operation may already be registered in the target stream line, causing a conflict with the separation column replacement process.
  • separation column replacement uses the same units as the analysis operation, separation column replacement and analysis operation cannot be performed simultaneously on the target streamline.
  • liquid chromatograph control method and liquid chromatograph according to this embodiment make it easier to avoid conflicts between the separation column replacement process and scheduled analysis operations.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Analytical Chemistry (AREA)
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PCT/JP2023/037573 2022-10-31 2023-10-17 液体クロマトグラフの制御方法および液体クロマトグラフ Ceased WO2024095765A1 (ja)

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JP2024554382A JPWO2024095765A1 (https=) 2022-10-31 2023-10-17
EP23885527.4A EP4614141A1 (en) 2022-10-31 2023-10-17 Method for controling liquid chromatograph and liquid chromatograph
CN202380072099.3A CN120019274A (zh) 2022-10-31 2023-10-17 液相色谱仪的控制方法以及液相色谱仪

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002530674A (ja) * 1998-11-20 2002-09-17 セピアテック ジーエムビーエイチ 物質を並列式の液体クロマトグラフィーで分離する装置および方法
US6641783B1 (en) * 1999-02-08 2003-11-04 Charles Pidgeon Chromatographic systems with pre-detector eluent switching
JP2013507614A (ja) * 2009-10-08 2013-03-04 ジーイー・ヘルスケア・リミテッド マルチストリーム高速液体クロマトグラフィーモジュール
JP2017161335A (ja) * 2016-03-09 2017-09-14 株式会社島津製作所 流体クロマトグラフ
WO2020171240A1 (ja) 2019-02-22 2020-08-27 株式会社日立ハイテク 分析装置
WO2020175510A1 (ja) * 2019-02-26 2020-09-03 株式会社日立ハイテク 液体クロマトグラフ分析装置、及びその制御方法
JP2022174101A (ja) 2017-01-03 2022-11-22 エルジー イノテック カンパニー リミテッド インダクタ及びこれを含むｅｍｉフィルター

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002530674A (ja) * 1998-11-20 2002-09-17 セピアテック ジーエムビーエイチ 物質を並列式の液体クロマトグラフィーで分離する装置および方法
US6641783B1 (en) * 1999-02-08 2003-11-04 Charles Pidgeon Chromatographic systems with pre-detector eluent switching
JP2013507614A (ja) * 2009-10-08 2013-03-04 ジーイー・ヘルスケア・リミテッド マルチストリーム高速液体クロマトグラフィーモジュール
JP2017161335A (ja) * 2016-03-09 2017-09-14 株式会社島津製作所 流体クロマトグラフ
JP2022174101A (ja) 2017-01-03 2022-11-22 エルジー イノテック カンパニー リミテッド インダクタ及びこれを含むｅｍｉフィルター
WO2020171240A1 (ja) 2019-02-22 2020-08-27 株式会社日立ハイテク 分析装置
WO2020175510A1 (ja) * 2019-02-26 2020-09-03 株式会社日立ハイテク 液体クロマトグラフ分析装置、及びその制御方法

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CN120019274A (zh) 2025-05-16
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