WO2020230284A1 - Chromatographe en phase liquide - Google Patents

Chromatographe en phase liquide Download PDF

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Publication number
WO2020230284A1
WO2020230284A1 PCT/JP2019/019222 JP2019019222W WO2020230284A1 WO 2020230284 A1 WO2020230284 A1 WO 2020230284A1 JP 2019019222 W JP2019019222 W JP 2019019222W WO 2020230284 A1 WO2020230284 A1 WO 2020230284A1
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WO
WIPO (PCT)
Prior art keywords
column
analysis
unit
configuration pattern
sample
Prior art date
Application number
PCT/JP2019/019222
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English (en)
Japanese (ja)
Inventor
浩志 大橋
大介 中山
Original Assignee
株式会社島津製作所
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 株式会社島津製作所 filed Critical 株式会社島津製作所
Priority to PCT/JP2019/019222 priority Critical patent/WO2020230284A1/fr
Priority to JP2021519195A priority patent/JP7259946B2/ja
Publication of WO2020230284A1 publication Critical patent/WO2020230284A1/fr

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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
    • G01N30/38—Flow patterns
    • G01N30/46—Flow patterns using more than one column
    • 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
    • G01N30/86—Signal analysis

Definitions

  • the present invention relates to a liquid chromatograph.
  • Multiple columns may be incorporated into the liquid chromatograph system.
  • there are various system configuration patterns such as a pattern in which all columns are connected in series, and a pattern in which the columns used for analysis are switched by a switching valve.
  • the present invention has been made in view of the above problems, and an object of the present invention is to enable accurate management of usage information of each column even when a plurality of columns are incorporated in a liquid chromatograph system. It is a thing.
  • the sample is fluidly connected to the liquid feed pump that feeds the mobile phase and downstream of the liquid feed pump, and the sample is placed in the analysis flow path through which the mobile phase from the liquid feed pump flows.
  • a sample injection section to be injected a sample separation section having at least one column fluidly connected downstream of the sample injection section on the analysis flow path, and a fluid downstream of the sample separation section on the analysis flow path.
  • a detector that is connected to the sample separation unit to detect the sample components separated in the sample separation unit, a column information storage unit that stores information used for analysis of each of the columns of the sample separation unit, and the sample separation unit.
  • the column used for the analysis was specified by using the configuration pattern holding unit that holds the configuration pattern of the column constituting the unit and the configuration pattern of the column held in the configuration pattern holding unit, and said. It includes a column information updating unit configured to update the usage information stored in the column information storage unit for the column used for the analysis.
  • the "constituent pattern" of the column constituting the sample separation section means how the column of the sample separation section is provided.
  • the system side holds the constituent pattern of the column constituting the sample separation unit, and recognizes the column used for analysis by using the constituent pattern. It is designed to do. Therefore, the usage information about the column used in the analysis can be accurately updated. As a result, even when a plurality of columns are incorporated in the system, usage information of each column can be accurately managed.
  • the liquid chromatograph of this embodiment includes a liquid feed pump 2, a sample injection unit 6, a sample separation unit 8, a detector 10, a control device 12, and a column information storage unit 14. There is.
  • the liquid feed pump 2 is for feeding the mobile phase in the analysis flow path 4.
  • the sample injection unit 6 injects a sample into the analysis flow path 4 through which the mobile phase fed by the liquid feed pump 2 flows.
  • the sample separation unit 8 is provided on the analysis flow path 4 downstream of the sample injection unit 6.
  • the sample separation unit 8 has at least one column 22 (see FIGS. 2 to 6) and a column oven (not shown) for adjusting the temperature of the column 22 to a predetermined temperature.
  • the sample injected into the analysis flow path 4 by the sample injection unit 6 is separated for each component in the sample separation unit 8.
  • the number of column ovens provided in the sample separation unit 8 is not limited to one.
  • all the columns 22 may be housed in one column oven, but each column 22 is dispersedly housed in a plurality of column ovens. You may.
  • the detector 10 is provided on the analysis flow path 4 downstream of the sample separation unit 8. The sample component separated by the sample separation unit 8 is detected by the detector 10.
  • the control device 12 is for controlling the operation of the liquid feed pump 2, the sample injection unit 6, the sample separation unit 8, and the detector 10.
  • the control device 12 may be realized by one computer, or may be realized by two or more computers (for example, a system controller and a personal computer electrically connected to the system controller). May be good.
  • the column information storage unit 14 is for storing usage information of each column 22 provided in the sample separation unit 8.
  • the usage information is mainly the number of times the column 22 has been used for analysis, but may include the cumulative usage time of the column 22.
  • the column information storage unit 14 can be realized by a memory module individually attached to the column 22. In that case, the memory module attached to each column 22 is connected to a communication port provided in the column oven accommodating the column 22 to which the memory module is attached, and electrically communicates with the column oven. Is done.
  • the column information storage unit 14 can also be realized by a part of the storage area of the information storage device provided in the control device 12 or a part of the storage area of the information storage device provided in the column oven.
  • the control device 12 includes a configuration pattern setting unit 16, a configuration pattern holding unit 18, and a column information updating unit 20.
  • the configuration pattern setting unit 16 and the column information update unit 20 are functions obtained by executing a predetermined program in the control device 12.
  • the configuration pattern holding unit 18 is a function realized by a part of the storage area of the information storage device provided in the control device 12.
  • the configuration pattern setting unit 16 is configured to set the configuration pattern of the column 22 in the sample separation unit 8 based on the information input from the user (system builder).
  • the configuration pattern of the column 22 in the sample separation unit 8 is how the column 22 is provided in the sample separation unit 8, and which column 22 is in which column oven when a plurality of column ovens are provided. It means that it is contained as such.
  • the configuration pattern setting unit 16 presents a plurality of configuration patterns as shown in FIGS. 2 to 6 to the user as candidates (hereinafter, pattern candidates), and the pattern candidates selected by the user from among those pattern candidates. Is configured to be set as a configuration pattern.
  • the configuration pattern holding unit 18 is configured to hold the configuration pattern set by the configuration pattern setting unit 16 as the configuration pattern of the sample separation unit 8.
  • the column information update unit 20 identifies the column 22 used for the analysis based on the configuration pattern held in the configuration pattern holding unit 18, and the column 22 used for the analysis.
  • Update usage information for. Updating usage information means increasing the number of times the column 22 used in the analysis is used by one when the usage information is the number of times it has been used for analysis, and when the usage information includes cumulative usage time. This means increasing the cumulative usage time of the column 22 used in the analysis by the time used.
  • the column information storage unit 14 is a memory module individually attached to each column 22, the usage information of the column information storage unit 14 is updated through the communication port of the column oven accommodating the column 22 used for the analysis. ..
  • the configuration pattern of FIG. 2 is a series configuration pattern in which a plurality of columns 22 are all connected in series. In such a series connection pattern, all columns 22 are used once the analysis is performed. Therefore, the column information update unit 20 updates the usage information stored in the column information storage unit 14 for all the columns 22 when one analysis is executed.
  • columns 22 may be any number. Further, not all columns 22 need to be housed in a common column oven, and may be distributed and housed in a plurality of column ovens.
  • the configuration patterns of FIGS. 3, 4 and 5 are all column switching patterns configured so that the column 22 used for analysis can be switched by the switching mechanism.
  • the flow path downstream of the sample injection unit 6 is connected to the common port of the multi-port valve 24 (switching mechanism), and each of the six columns 22 is connected to the selection port of the multi-port valve 24.
  • the column 22 used for analysis is selectively switched depending on the position of the multi-port valve 24.
  • the column information updating unit 20 uses the information about the configuration pattern every time the analysis is executed, and multiports at the time of the analysis. Which column 22 is used is recognized from the position of the valve 24, and the usage information stored in the column information storage unit 14 is updated for the column 22 used for the analysis.
  • the number of columns 22 may be any number. Further, not all columns 22 need to be housed in a common column oven, and may be distributed and housed in a plurality of column ovens. Further, in FIG. 3, one column 22 is connected to each selection port of the multi-port valve 24, but even if a plurality of columns 22 connected in series to each selection port of the multi-port valve 24 are connected. Good.
  • the column 22 used for analysis is selectively switched by a switching mechanism including a two-position valve 26 and two multi-port valves 28 and 30.
  • a column 22 is connected to each of the six select ports of the multiport valves 28 and 30.
  • Each common port of the multi-port valves 28 and 30 is connected to one port of the two-position valve 26, respectively.
  • the flow path downstream of the sample injection unit 6 is connected to one port of the 2-position valve 26, and either the multi-port valve 28 side or the multi-port valve 30 side is selected depending on the position of the 2-position valve 26. ..
  • the multiport valve 28 side is selected, any one of the six columns 22 connected to the selection port of the multiport valve 28 is used for analysis and the multiport valve 30 side is selected.
  • any one of the six columns 22 connected to the selected port of the multi-port valve 30 is used for the analysis.
  • the column information updating unit 20 uses the information about the configuration pattern every time the analysis is executed, and multiports at the time of the analysis. It recognizes which column 22 is used from the positions of the valves 26, 28, and 30, and updates the usage information stored in the column information storage unit 14 for the column 22 used for the analysis.
  • the number of columns 22 connected to the multi-port valves 28 and 30 in FIG. 4 may be any number. Further, all the columns 22 may be housed in a common column oven, but the column 22 connected to the multi-port valve 28 and the column 22 connected to the multi-port valve 30 are in separate column ovens. It may be contained. Further, in FIG. 4, one column 22 is connected to each selection port of the multi-port valves 28 and 30, but a plurality of columns 22 connected in series to each selection port of the multi-port valves 28 and 30 are connected. May be connected.
  • the column 22 used for analysis is selectively switched depending on the position of the 2-position valve 32 (switching mechanism).
  • the column information updating unit 20 uses the information about the configuration pattern to perform two positions at the time of the analysis each time the analysis is executed. It recognizes which side of the column 22 is used from the position of the valve 32, and updates the usage information stored in the column information storage unit 14 for the column 22 used for the analysis.
  • one column 22 is configured to be used for analysis depending on the position of the two-position valve 32, but a plurality of columns connected in series at at least one position of the two-position valve 32.
  • Column 22 may be configured to be used for analysis. Further, all the columns 22 may be housed in a common column oven, but may be distributed and housed in a plurality of column ovens.
  • the configuration pattern of FIG. 6 is a pattern in which a plurality of columns 22 are dispersed and provided on different analysis flow paths 4a and 4b.
  • the mobile phase fed by the liquid feed pump 2a flows through the analysis flow path 4a, and the mobile phase fed by the liquid feed pump 2b flows through the analysis flow path 4b.
  • the injection of the sample into the analysis channels 4a and 4b is performed by the common sample injection unit 6.
  • Detectors 10a and 10b are provided downstream of the sample separation section 8 on the analysis channels 4a and 4b, respectively.
  • the sample injection unit 6 includes an injection port for injecting a sample into the analysis flow path 4a and an injection port for injecting a sample into the analysis flow path 4b, and the sample injection unit 6 performs a sample injection operation.
  • the analysis is executed in any of the analysis channels 4a and 4b, or the same sample is simultaneously analyzed in both analysis channels 4a and 4b by the sample injection operation of the sample injection unit 6. It is configured to be selected.
  • the column information updating unit 20 uses the information about the configuration pattern to perform the analysis every time the analysis is executed. Recognizing whether it was executed in 4a or 4b or in both analysis channels 4a and 4b, the column information storage unit 14 stores the column 22 provided on the analysis channel in which the analysis was executed. Update the usage information that has been done.
  • one separation column 22 is provided in each of the analysis flow paths 4a and 4b, but a plurality of separation columns 22 are provided in at least one of the analysis flow paths 4a and 4b. May be good. Further, the separation columns 22 on the analysis channels 4a and 4b may be housed in a common column oven or may be housed in separate column ovens.
  • the control device 12 sends an analysis start instruction to the sample injection unit 8.
  • the sample injection unit 8 executes sample injection into the analysis flow path 4 (step 101).
  • the column information updating unit 20 of the control device 12 identifies the column 22 used (or used) for the analysis from the configuration pattern of the sample separation unit 8 held in the configuration pattern holding unit 18 (step). 102), the usage information stored in the column information storage unit 14 for the specified column 22 is updated (step 103). For example, when the configuration pattern is a series configuration pattern as shown in FIG. 2, the column information update unit 20 identifies all columns 22 as columns 22 used (or used) for analysis.
  • the usage information for all columns 22 is updated when the sample injection is performed or after the sample injection is performed.
  • the configuration pattern is a column selection pattern as shown in FIGS. 3 to 5
  • the column information update unit 20 is used for analysis from the position of each valve constituting the switching mechanism.
  • the column 22 (or used) is identified and the usage information of the column 22 used (or used) for the analysis is updated when the sample injection is performed or after the sample injection is performed.
  • the configuration pattern is the analysis flow path selection pattern as shown in FIG. 6, the column information update unit 20 is used for analysis from the injection port into which the sample is injected in the sample injection unit 6.
  • the column 22 (or used) is identified and the usage information of the column 22 used (or used) for the analysis is updated when the sample injection is performed or after the sample injection is performed.
  • the usage information is the number of times the column 22 has been used, the number of times the column 22 has been used is increased by one. After the analysis is completed, if there is a sample to be analyzed next, the operations of steps 101 to 103 are executed in the next analysis.
  • Embodiments of the liquid chromatograph according to the present invention are as follows.
  • liquid chromatograph in the analysis flow path in which the liquid feed pump that feeds the mobile phase and the liquid feed pump are fluidly connected downstream of the liquid feed pump and the mobile phase from the liquid feed pump flows.
  • a sample injection section for injecting a sample into a sample a sample separation section having at least one column fluidly connected downstream of the sample injection section on the analysis flow path, and a downstream of the sample separation section on the analysis flow path.
  • a detector that is fluidly connected to the sample separation unit and detects the sample components separated in the sample separation unit, and a column information storage unit that stores information used for analysis of each of the columns of the sample separation unit.
  • the configuration pattern holding unit that holds the configuration pattern of the column that constitutes the sample separation unit and the configuration pattern of the column that is held in the configuration pattern holding unit. It also includes a column information updating unit configured to update the usage information stored in the column information storage unit for the column used in the analysis.
  • one pattern candidate selected from a plurality of pattern candidates prepared in advance is selected as the constituent pattern of the column constituting the sample separation unit.
  • the configuration pattern setting unit is provided with a configuration pattern setting unit configured to be set, and the configuration pattern holding unit holds a pattern candidate set by the configuration pattern setting unit as the configuration pattern. According to such an aspect, when constructing the system of the liquid chromatograph, the work of registering the constituent pattern of the sample separation part in the system becomes easy.
  • the pattern candidate there is a series configuration pattern in which all of the plurality of columns are connected in series, and the column information update unit is held by the configuration pattern holding unit.
  • the configuration pattern is the series configuration pattern, the usage information stored in the column information storage unit is updated for all the columns every time the analysis is executed.
  • the pattern candidate there is a column switching pattern configured to switch the column used for analysis from among the plurality of columns by a switching mechanism, and the column information update unit Recognizes the column used in the analysis based on the switching operation of the switching mechanism when the configuration pattern held in the configuration pattern holding unit is the column switching pattern, and is used in the analysis.
  • the column is configured to update the usage information stored in the column information storage unit.
  • the columns are provided in each of the analysis channels, and the sample injection section is any one of them.
  • There is an analysis flow path switching pattern configured to inject a sample into the analysis flow path, and in the column information update unit, the configuration pattern held in the configuration pattern holding unit is the analysis flow path switching pattern.
  • the column provided in the analysis flow path into which the sample is injected by the sample injection unit is recognized as the column used for the analysis, and the column information storage for the column used for the analysis. It is configured to update the usage information stored in the unit.
  • the first to third aspects of the first aspect can be freely combined with each other.
  • the column information storage unit is a memory module individually attached to the column. This second aspect can be combined with the first aspect.
  • a column oven for accommodating the column inside and adjusting the temperature of the column to a predetermined temperature, and the column oven is attached to all the columns housed inside.
  • the column information update unit is provided with a communication port for performing electrical communication with the memory module, and the column information update unit is stored in the memory module via the communication port of the column oven.
  • An example is that it is configured to update information.
  • the usage information is the number of times the column has been used for analysis.
  • This third aspect can be freely combined with the first aspect and the second aspect.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
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  • Sampling And Sample Adjustment (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

L'invention concerne un chromatographe en phase liquide comprenant : une pompe d'alimentation en liquide (2) qui alimente une phase mobile; une unité d'injection d'échantillon (6) qui est en liaison fluidique avec un côté aval de la pompe d'alimentation en liquide (2) et qui injecte un échantillon dans un canal d'analyse (4) à travers lequel s'écoule la phase mobile provenant de la pompe d'alimentation en liquide (2); une unité de séparation d'échantillon (8) qui comporte au moins une colonne (22) en liaison fluidique avec un côté aval de l'unité d'injection d'échantillon (6) sur le canal d'analyse (4); un détecteur (10) qui est en liaison fluidique avec un côté aval de l'unité de séparation d'échantillon (8) sur le canal d'analyse (4) et qui détecte un composant d'échantillon séparé dans l'unité de séparation d'échantillon (8); une unité de stockage d'informations de colonne (14) qui stocke des informations d'utilisation pour l'analyse de chacune des colonnes (22) de l'unité de séparation d'échantillon (8); une unité de maintien de schéma de configuration (18) qui maintient un schéma de configuration des colonnes (22) constituant l'unité de séparation d'échantillon (8); et une unité de mise à jour d'informations de colonne (20) configurée pour reconnaître les colonnes (22) utilisées dans l'analyse à l'aide du schéma de configuration, des colonnes (22), maintenue dans l'unité de maintien de schéma de configuration (18), et mettre à jour les informations d'utilisation stockées dans l'unité de stockage d'informations de colonne (14) pour les colonnes (22) utilisées dans l'analyse.
PCT/JP2019/019222 2019-05-15 2019-05-15 Chromatographe en phase liquide WO2020230284A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/JP2019/019222 WO2020230284A1 (fr) 2019-05-15 2019-05-15 Chromatographe en phase liquide
JP2021519195A JP7259946B2 (ja) 2019-05-15 2019-05-15 液体クロマトグラフ

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PCT/JP2019/019222 WO2020230284A1 (fr) 2019-05-15 2019-05-15 Chromatographe en phase liquide

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115808489A (zh) * 2022-07-06 2023-03-17 胡威 一种基于层析纯化的连续纯化装置和方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6454350A (en) * 1987-08-26 1989-03-01 Japan Spectroscopic Co Separation column for chromatograph and administration device thereof
JPH09171022A (ja) * 1995-10-31 1997-06-30 Hewlett Packard Co <Hp> 分析測定装置における交換可能な部品を識別する装置
JP2011220789A (ja) * 2010-04-08 2011-11-04 Hitachi High-Technologies Corp 液体クロマトグラフ装置
EP2581741A1 (fr) * 2011-10-12 2013-04-17 Agilent Technologies, Inc. Transfert de méthodes en geleant un paramètre initialement non contrôlé
WO2018189871A1 (fr) * 2017-04-13 2018-10-18 株式会社島津製作所 Procédé d'analyse d'échantillon utilisant un couplage chromatographie liquide-spectrométrie de masse
JP2018173302A (ja) * 2017-03-31 2018-11-08 株式会社日立ハイテクサイエンス 液体クロマトグラフ装置

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6454350A (en) * 1987-08-26 1989-03-01 Japan Spectroscopic Co Separation column for chromatograph and administration device thereof
JPH09171022A (ja) * 1995-10-31 1997-06-30 Hewlett Packard Co <Hp> 分析測定装置における交換可能な部品を識別する装置
JP2011220789A (ja) * 2010-04-08 2011-11-04 Hitachi High-Technologies Corp 液体クロマトグラフ装置
EP2581741A1 (fr) * 2011-10-12 2013-04-17 Agilent Technologies, Inc. Transfert de méthodes en geleant un paramètre initialement non contrôlé
JP2018173302A (ja) * 2017-03-31 2018-11-08 株式会社日立ハイテクサイエンス 液体クロマトグラフ装置
WO2018189871A1 (fr) * 2017-04-13 2018-10-18 株式会社島津製作所 Procédé d'analyse d'échantillon utilisant un couplage chromatographie liquide-spectrométrie de masse

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115808489A (zh) * 2022-07-06 2023-03-17 胡威 一种基于层析纯化的连续纯化装置和方法

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JPWO2020230284A1 (fr) 2020-11-19

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