WO2020230284A1

WO2020230284A1 - Liquid chromatograph

Info

Publication number: WO2020230284A1
Application number: PCT/JP2019/019222
Authority: WO
Inventors: 浩志大橋; 大介中山
Original assignee: 株式会社島津製作所
Priority date: 2019-05-15
Filing date: 2019-05-15
Publication date: 2020-11-19
Also published as: JPWO2020230284A1; JP7259946B2

Abstract

This liquid chromatograph comprises: a liquid feeding pump (2) that feeds a mobile phase; a sample injection unit (6) that is fluidly connected to a downstream side of the liquid feeding pump (2) and injects a sample into an analysis channel (4) through which the mobile phase from the liquid feeding pump (2) flows; a sample separation unit (8) that has at least one column (22) fluidly connected to a downstream side of the sample injection unit (6) on the analysis channel (4); a detector (10) that is fluidly connected to a downstream side of the sample separation unit (8) on the analysis channel (4) and detects a sample component separated in the sample separation unit (8); a column information storage unit (14) that stores use information for the analysis of each of the columns (22) of the sample separation unit (8); a configuration pattern holding unit (18) that holds a configuration pattern of the columns (22) constituting the sample separation unit (8); and a column information update unit (20) configured to recognize the columns (22) used in the analysis using the configuration pattern, of the columns (22), held in the configuration pattern holding unit (18), and update the use information stored in the column information storage unit (14) for the columns (22) used in the analysis.

Description

Liquid chromatograph

The present invention relates to a liquid chromatograph.

In liquid chromatography analysis, the separation ability by the column has a great influence on the analysis result. Since the separation medium filled in the column deteriorates and the separability decreases as the cumulative usage time increases, it is necessary to properly manage the usage status of the column.

Therefore, it has been proposed and implemented to attach a memory module that stores usage information such as the last usage date and time, cumulative usage time, and number of usages of the column to each column so that information management regarding the column can be performed appropriately and easily. (See, for example, Patent Document 1).

Japanese Unexamined Patent Publication No. 2008-209327

Multiple columns may be incorporated into the liquid chromatograph system. In that case, 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.

In the conventional liquid chromatograph system, when multiple columns are incorporated into the system as described above, how to manage the usage information of each column is not considered. Therefore, when multiple columns are installed in the system, it is impossible to know which columns are used in the analysis and which columns are not used, and to accurately manage the usage information of each column. Met.

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.

In the liquid chromatograph according to the present invention, 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.

Here, the "constituent pattern" of the column constituting the sample separation section means how the column of the sample separation section is provided.

In the liquid chromatograph according to the present invention, 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.

It is a schematic block diagram which shows one Example of the liquid chromatograph. It is a figure which shows roughly an example of the structural pattern of the sample separation part of the same Example. It is a figure which shows the other example of the structural pattern of the sample separation part of the same Example schematicly. It is a figure which shows the other example of the structural pattern of the sample separation part of the same Example schematicly. It is a figure which shows the other example of the structural pattern of the sample separation part of the same Example schematicly. It is a figure which shows the other example of the structural pattern of the sample separation part of the same Example schematicly. It is a flowchart which shows an example of the update operation of the column usage information in the same Example.

Hereinafter, an example of the liquid chromatograph according to the present invention will be described with reference to the drawings.

As shown in FIG. 1, 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.

Note that the number of column ovens provided in the sample separation unit 8 is not limited to one. When the sample separation unit 8 has a plurality of columns 22, 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. As a typical configuration pattern of the column 22, the ones shown in FIGS. 2 to 6 exist. 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.

When the analysis of the sample is executed, 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. When 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. ..

A typical configuration pattern of the sample separation unit 8 shown in FIGS. 2 to 6 will be described.

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.

Although six columns 22 are provided in FIG. 2, 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.

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.

In the configuration pattern of FIG. 3, 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. There is. In this configuration, the column 22 used for analysis is selectively switched depending on the position of the multi-port valve 24. When the configuration pattern holding unit 18 of the control device 12 holds information about this configuration pattern, 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.

Although six columns 22 are provided in FIG. 3, 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.

In the configuration pattern of FIG. 4, 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. .. When 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. At that time, any one of the six columns 22 connected to the selected port of the multi-port valve 30 is used for the analysis. When the configuration pattern holding unit 18 of the control device 12 holds information about this configuration pattern, 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.

Although six columns 22 are connected to each of the

multi-port valves

28 and 30 in FIG. 4, the number of columns 22 connected to the

multi-port valves

28 and 30, respectively, 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.

In the configuration pattern of FIG. 5, the column 22 used for analysis is selectively switched depending on the position of the 2-position valve 32 (switching mechanism). When the configuration pattern holding unit 18 of the control device 12 holds information about this configuration pattern, 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.

In FIG. 5, 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. When the configuration pattern holding unit 18 of the control device 12 holds information about this configuration pattern, 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.

In FIG. 6, 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.

An example of the operation of updating the usage information of the column 22 of the sample separation unit 8 will be described with reference to the flowchart of FIG. 7 together with FIG.

When it is time to start the analysis of the sample, the control device 12 sends an analysis start instruction to the sample injection unit 8. Upon receiving the analysis start instruction, the sample injection unit 8 executes sample injection into the analysis flow path 4 (step 101). At this time, 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. When 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. Further, when 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. If 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.

The examples described above are merely examples of embodiments of the liquid chromatograph according to the present invention. Embodiments of the liquid chromatograph according to the present invention are as follows.

In the embodiment of the liquid chromatograph according to the present invention, 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. Recognize the column used for analysis by using 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.

In the first aspect of the above embodiment of the liquid chromatograph according to the present invention, 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.

In the first aspect of the first aspect, as 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. When 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.

In the second aspect of the first aspect, as 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.

In the third aspect of the first aspect, there are a plurality of the analysis channels as the pattern candidates, 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. When is, 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.

In the second aspect of the above embodiment of the liquid chromatograph according to the present invention, the column information storage unit is a memory module individually attached to the column. This second aspect can be combined with the first aspect.

As a specific example of the second aspect, a column oven for accommodating the column inside and adjusting the temperature of the column to a predetermined temperature is provided, 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.

In the third aspect of the above embodiment of the liquid chromatograph according to the present invention, 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.

2,2a, 2b Liquid feed pump 4,4a, 4b Analytical flow path 6 Sample injection unit 8

Sample separation unit

10, 10a, 10b Detector 12 Controller 12 Control device 14 Column information storage unit 16 Configuration pattern setting unit 18 Configuration pattern holding unit 20 Column information updater 22

Columns

24, 28, 30 Multi-port valve (switching mechanism)
26,32 2 position valve (switching mechanism)

Claims

A liquid feed pump that feeds the mobile phase and
A sample injection unit that is fluidly connected downstream of the liquid feed pump and injects a sample into an analysis flow path through which a mobile phase from the liquid feed pump flows.
A sample separation section having at least one column fluidly connected downstream of the sample injection section on the analysis flow path,
A detector fluidly connected to the downstream of the sample separation section on the analysis flow path and detecting the sample components separated in the sample separation section,
A column information storage unit that stores information used for analysis of each of the columns of the sample separation unit, and a column information storage unit.
A configuration pattern holding unit that holds the configuration pattern of the column that constitutes the sample separation unit,
The column used in the analysis is identified by using the configuration pattern of the column held in the configuration pattern holding unit, and the column used in the analysis is stored in the column information storage unit. A liquid chromatograph comprising a column information updater configured to update information.
As the configuration pattern of the column constituting the sample separation unit, a configuration pattern setting unit configured to set one pattern candidate selected from a plurality of pattern candidates prepared in advance is provided.
The liquid chromatograph according to claim 1, wherein the configuration pattern holding unit holds a pattern candidate set by the configuration pattern setting unit as the configuration pattern.
As the pattern candidate, there is a series configuration pattern in which all of the plurality of columns are connected in series.
When the configuration pattern held in the configuration pattern holding unit is the series configuration pattern, the column information update unit stores all the columns in the column information storage unit every time the analysis is executed. The liquid chromatograph according to claim 2, which is configured to update the usage information.
As 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.
When the configuration pattern held in the configuration pattern holding unit is the column switching pattern, the column information updating unit identifies and analyzes the column used for analysis based on the switching operation of the switching mechanism. The liquid chromatograph according to claim 2, wherein the usage information stored in the column information storage unit is updated for the column used in the above.
As the pattern candidate, there are a plurality of the analysis channels, each of the analysis channels is provided with the column, and the sample injection unit puts a sample in any one or a plurality of the analysis channels. There is an analytical flow path switching pattern that is configured to inject
The column information update unit is provided in the analysis flow path in which the sample is injected by the sample injection unit when the configuration pattern held in the configuration pattern holding unit is the analysis flow path switching pattern. The second aspect of the present invention, wherein the column is recognized as the column used for the analysis, and the usage information stored in the column information storage unit is updated for the column used for the analysis. Liquid chromatograph.
The liquid chromatograph according to claim 1, wherein the column information storage unit is a memory module individually attached to the column.
A column oven for accommodating the column inside and adjusting the temperature of the column to a predetermined temperature is provided.
The column oven comprises a communication port for conducting electrical communication with the memory module attached to all the columns housed therein.
The liquid chromatograph according to claim 6, wherein the column information updating unit is configured to update the usage information stored in the memory module via the communication port of the column oven.
The liquid chromatograph according to claim 1, wherein the usage information is the number of times the column has been used for analysis.