JP2012237635A - Program for chromatograph - Google Patents

Abstract

PROBLEM TO BE SOLVED: To alleviate a cumbersome and complicated setting of each equipment configuring a high performance liquid chromatograph and to integrate data output from a detector.SOLUTION: A plurality of communication interfaces are used for communication between a computer 80 and respective equipment configuring a chromatograph related machine. The chromatograph related machine includes a plurality of detectors 74 and 76 which output, in parallel, chromatograms with respective time axes adjusted even when formats thereof output from respective detectors differ. When column units are serially arranged, the chromatograms are output with a correction of a detection delay due to a difference in flow channel length between the detector for a preceding stage and the detector for a subsequent stage.

Description

  The present invention relates to an integrated program for chromatographs, and more particularly to improvement of a program for integrating a plurality of chromatograms output from a chromatograph.

Conventionally, a high performance liquid chromatograph (HPLC) has been used to perform separation analysis and fractionation of a target component in a mixture. A chromatogram can be obtained in a short time by measuring with a high-speed liquid chromatograph. The obtained chromatogram is used for qualitative analysis and quantitative analysis.
As shown in FIG. 6, a general high performance liquid chromatograph has a high performance liquid chromatograph 60 including a pump 62, an autosampler 66, a column oven 70, and a plurality of detectors 74 and 76. Prepare.
When many related devices are connected in this way, the communication interface may be different for each related device. As an example, the communication interface between the computer 80 and each device includes ATAPI 65, USB 69, SCSI 75, and RS-232C77.
As described above, in the high performance liquid chromatograph, a large number of devices are used as related devices, the standards of communication interfaces thereof are different, and the communication speed between the computer and each device may be different.

Further, not only the communication interface but also the user interface for displaying the setting value and the measurement result of each device may be different. When a plurality of different types of detectors are connected, chromatograms are output in different formats for each detector. The output chromatograms are not only two-dimensional but also three-dimensional, and even in the same two-dimensional chromatogram, the time (X-axis) scale is different.
When multiple chromatograms are output to different screens in this way, the operator must compare the retention times and peak areas while referring to the time axes of the respective chromatograms, and compare each chromatogram. Is complicated.

Further, when a plurality of detectors are provided and these detectors are connected in series behind the column unit, a flow path difference occurs in each of the detectors. For example, in FIG. 6, the detector 74 is connected to the front stage of the flow path, and the detector 76 is connected to the subsequent stage, and detection by the detector 76 is delayed due to the flow path difference from the detector 74.
When the detectors are connected in series behind the column unit in this way, the detection delay due to the flow path difference between the detectors must be taken into account, which further increases the complexity.

On the other hand, since many setting screens are displayed for each device on the operation terminal, the operator inputs setting values in the setting item field for each device, but the setting screen is switched for each device. Entering a value is cumbersome.
In addition, there are various models and versions even if one device is used. If the manufacturer is different, the setting method is greatly different. Even if the manufacturer is the same, if the version is different, the setting method is quite different. For this reason, the operator has to make a setting with the model / version in mind, which is complicated.

Furthermore, there may be a case where a plurality of chromatograph-related devices are connected in series and the subsequent device must be set in consideration of the operation of the previous device. Although it is possible to set each detector by switching the individual setting screen, there is no means to comprehensively manage the settings of each detector, so when setting the previous device, the operation of the subsequent device can be changed. In some cases, the influence must be taken into account, which causes troublesome setting of each device. For example, when a column unit is connected to the subsequent stage of the switching valve, the measurement wavelength of the detector must be changed at a predetermined timing after the switching valve is operated, and the setting of the detector becomes complicated.
As described above, there is a need for means for alleviating the complexity and complexity of integration of chromatograms output from detectors used in high performance liquid chromatographs and the setting of each device.

  The present invention has been made in view of the problems relating to the integration (input) of each device and the integration of data output from the detector, as seen in the prior art, and its purpose is to constitute a high-performance liquid chromatograph. The purpose is to reduce the complexity and complexity of the setting of each device, and to integrate the data output obtained from the detector.

In order to make it easy to see chromatograms output from a plurality of detectors of different models / versions as a result of extensive studies by the present inventors, the inventors have adjusted the time axis of chromatograms and the flow path difference between column units. We thought that it was necessary to integrate the output from the detector, such as the correction of the detection delay due to.
In addition, in order to alleviate the complexity and complexity of the setting of each device, we thought that it was necessary to unify the input format of the setting of each device used in the liquid chromatograph. For that purpose, the information entered by the operator from the setting screen is organized, and each device is set by performing appropriate operations on each device based on the entered information. Need to fill.

According to the chromatograph integration program according to the present invention, in order to integrate chromatograms output from a plurality of detectors included in a chromatograph-related device, a two-dimensional chromatogram or a three-dimensional chromatogram output from each detector. The time axis scale of grams is unified and displayed in parallel.
That is, as described in claim 1,
In an integrated program that integrates chromatograph-related instruments having independent control programs and configuration files,
Chromatographic equipment
A column unit that separates substances into components using the difference in physical properties of substances contained in the sample;
Two or more detectors connected to the rear of the column unit,
Each chromatograph-related device is connected to the control computer via the communication interface of each standard,
It comprises an output integration mechanism that converts the output information of each detector into a desired unit, unifies the time axis scale, and displays two or more two-dimensional chromatograms or three-dimensional chromatograms in parallel. .
Further, as described in claim 2, a two-dimensional chromatograph having a specific wavelength may be extracted from the three-dimensional chromatogram.

When two or more detectors are connected in series behind the column unit, there is a flow path difference between the upstream detector and the downstream detector, so that a detection delay occurs in the downstream detector. In this case, it is necessary to consider this detection delay when displaying the chromatograms output from the respective detectors in parallel. Therefore, it was decided to correct the detection delay of the chromatogram output from the subsequent detector.
That is, as described in claim 3,
The two or more detectors are connected in series behind the column unit,
It is preferable that the output integration mechanism corrects a detection delay due to a flow path difference between the upstream detector and the downstream detector connected in series.

A large number of chromatograph-related devices are connected to the computer, but when initializing them, it is usually necessary to launch a setting screen separately and input settings for each.
The setting items of a plurality of chromatograph-related devices can be displayed on one screen by using the chromatograph integration program according to the present invention. This is preferable because the operator can set each chromatograph-related device without switching the setting screen.
On the other hand, the model and version of each chromatograph-related device are often different, and the input format may be different for each model / version. Even when the model and version are different, it is preferable to display the setting item column in the same format so that the operator can set each device without being aware of it.
That is, the present invention as described in claim 4,
The integrated program includes a user interface display mechanism for displaying a user interface for collectively displaying setting items of each device in one setting item column;
A model that determines the model / version of each device by connecting the two or more devices to the control computer, selects the setting items necessary for each device, and provides information related to the setting items to the user interface display mechanism It is preferable to further include a version discrimination mechanism.
In addition, as described in claim 5,
The integrated program allows the setting of each device to be input in the desired unit on the user interface by the control program even when the model / version of each device is different, and corresponds to the setting items of each device Therefore, it is preferable to have a setting unit integration mechanism that performs unit conversion by converting the information input to the user interface into units.

When a plurality of chromatograph-related devices are connected in series and these operations are linked, it is preferable to integrate the settings of each device. In order to integrate the settings of a plurality of linked devices, it is preferable to further provide a response time item as an item for setting the operation timing of the device in the setting item column of the user interface. If this response time is set, the subsequent device can be operated after the response time has elapsed with the timing at which the operation timing of the previous device starts or ends as a base point.
That is, as described in claim 6,
A setting item displayed as a user interface by the user interface display mechanism is further provided with a setting item relating to operation timing control between the chromatograph-related devices, and the operation of a device is set by setting the operation timing of the interlocking device. The setting related to the operation timing of the other device according to the information input to the setting item related to the control of the operation timing based on the timing at which the operation of the device starts or ends so that the other device responds appropriately Is preferably performed.

In order to reflect the setting information input in the setting item column by the operator to each device, the setting information must be reflected to each device by some method.
The integrated program according to the present invention reflects the setting by the following method.
For example, as described in claim 7,
It is preferable that each detector is set by starting a setting program for each detector, starting up a user interface of each chromatograph-related device, and inputting setting information on the user interface.
For example, as described in claim 8,
It is preferable to set each detector by directly rewriting the setting file of each detector.
For example, as described in claim 9,
It is preferable to set each device by inputting the setting value in the setting item column of each device by performing the same operation as the keyboard operation on the setting screen of each device.

Two or more detectors are connected to the rear of the column unit as a chromatograph-related device, and each chromatogram output from each detector is displayed in parallel based on the time axis. By using the chromatograph integration program according to the present invention, the time axis scale of the two-dimensional and three-dimensional chromatograms is adjusted.
At this time, a detector may be connected in series behind the column unit. Even in such a case, the flow difference between the upstream detector and the downstream detector is taken into consideration, and the chromatogram output from the downstream detector is corrected as a detection delay.

In addition, the setting information input in the setting item column using the chromatograph integration program according to the present invention is once stored in the temporary area, and the control program sets each device based on the setting information. Even if there is a difference in model due to different manufacturers of each device, or even when the manufacturer is the same, the manufacturing time is different, so even if the setting method is different due to different versions, the setting screen is not much You can input in the same format without change. The operator does not need to be aware of the difference in model / version when setting, and it is now possible to set each device simply by filling the setting item column.
Furthermore, we decided to automatically determine the model and version of the equipment connected to the control computer. By extracting necessary setting items for each device based on the model / version information and listing them on the user interface as setting item columns, the operator can use different models / versions in the measurement. Necessary setting items can be confirmed at a glance.
Even if some of the connected devices are changed, there are some changes in the number of setting items in the setting item column and the unit of setting values due to differences in model and version, but the change is minimized. Since all devices can be set with almost the same procedure, the complexity of setting is reduced.

  Furthermore, even when chromatograph-related devices are connected in series, a response time item is separately provided in the setting item column, so when making settings related to the operation of the subsequent device, be aware of the relationship with the previous device. This eliminates the need for setting and reduces the complexity of setting.

It is the figure which showed the processing structure when setting each apparatus of the chromatograph integrated program of this invention. It is the figure which showed the process sequence of the chromatograph integrated program of this invention as the flowchart. It is the figure which showed a mode that the information regarding the apparatus connected by the model / version discrimination mechanism which concerns on this invention was displayed on the model / version display screen. It is the figure which showed the setting screen when the setting item of each apparatus is collectively displayed by the user interface display mechanism which concerns on this invention. It is the figure which showed the normal setting screen (when not using the chromatograph integrated program of this invention) when a PDA detector is connected to the control computer. It is the figure which showed the structure of a chromatograph related apparatus, the processing structure of a control program, and the communication interface of a chromatograph related apparatus and a main processing means. It is the figure which showed a mode when the several output chromatogram was displayed in parallel centering on elapsed time. It is explanatory drawing which showed the process of the chromatogram displayed in the various format from a some detector. It is explanatory drawing when the some chromatogram output from a some detector is displayed in parallel. A schematic diagram showing a conventional example (upper part) showing how measurement results output from each device are displayed on a plurality of screens, and a state (lower part) displaying measurement results on one screen according to the present invention. is there. It is the figure which arranged the chromatogram output from each detector in the vertical direction, and demonstrated delay time. It is the figure which showed a mode that the scale adjustment of the X-axis (elapsed time) of each chromatogram was performed.

Hereinafter, a preferred embodiment of the present invention will be described with reference to the drawings.
FIG. 1 shows a schematic configuration of a chromatograph integration program according to an embodiment of the present invention.
The integrated program 10 shown in FIG. 1 completes the setting of each device using the setting screen (user interface) 12 that collectively displays the setting item fields of each connected device and the information input on the setting screen as setting information. Models such as a temporary area 14 for temporarily storing, a control program 16 for referring to the recorded setting information for each device and inputting the setting information, and a pump, autosampler, detector, etc. connected to the control computer 20 And a model / version discriminating mechanism 18 for discriminating the version and a user interface display mechanism 19 for collectively displaying setting items corresponding to the model / version of each device on the setting screen.

  The model / version discriminating mechanism 18 discriminates the model and version of the device connected to the control computer 20, and setting items necessary for setting each model are displayed on the setting screen 12 as a setting item column by the user interface display mechanism 19. Are displayed together. Information input in the setting item column is temporarily stored in the temporary area 14 as setting information. Then, the control program 16 refers to the temporary area 14 of each device and reflects the setting information in the setting of each model.

  FIG. 2 is a flowchart showing the processing procedure of the chromatograph integration program according to the present invention. The chromatograph integration program 10 checks the model / version of each device currently connected by the model / version discrimination mechanism 18 (S10). Next, based on the model / version information of each device, information on setting items necessary for setting each device is selected by the model / version discrimination mechanism, and this information is sent to the user interface display mechanism 19. The user interface display mechanism 19 collectively displays setting items necessary for setting each device on the setting screen 12 as a setting item column (S12). When a setting value is input to the setting item column by the operator (S14), this setting value is stored as setting information in the temporary area 14 (S15). The control program 16 refers to the temporary area 14 (S16), and sets each device based on the setting information stored in the temporary area 14 (S18).

Next, each processing procedure shown in the flowchart will be described in more detail.
FIG. 3 shows a model / version display screen 30. This screen shows the model / version information of each currently connected device checked by the model / version discrimination mechanism 18.
Information on setting items required for each model / version is recorded in a file or database. The model / version discriminating mechanism searches the database and provides the user interface display mechanism 19 with information necessary for setting each device. Then, the user interface display mechanism 19 displays a setting item column for each device on the setting screen 12.

The types of each device constituting the chromatograph are listed in the device type display column 34. Among these devices, devices connected to the control computer are displayed in the connection state display box 32, and devices not connected are displayed in white. Further, when a device is connected to the control computer, the model name is displayed in the model name display field 36.
For example, according to the model / version display screen 30 in FIG. 3, the autosampler is in a connected state because the connection state display box 32 is filled and displayed, and the model name is “AS−” from the model name display field 36. 2059 ". On the other hand, the column oven is not connected because the connection state display box 32 is not filled.
If the model / version is unregistered but the model is not registered, the connection status display box 32 is filled and “unknown” is displayed in the model name display field 36.

The display of the setting screen will be described.
FIG. 4 shows a setting screen 40 for each device. Tabs are displayed on the setting screen 40 as many as the number of connected devices, and the operator can set each device by selecting the tab.
The setting items displayed differ depending on the model and version. In order to collect information necessary for setting each device, the model / version discriminating mechanism 18 searches a database or the like in advance, and the user interface display mechanism 19 receives information on the setting items of the model / version. The user interface display mechanism 19 displays setting items corresponding to the model / version on the setting screen 40.
For example, in FIG. 4, the PDA detector tab 42a is currently selected, and setting items corresponding to the tab 42a are listed. In an actual PDA detector, the sensitivity can be set by selecting a radio button because the sensitivity can be set in three stages of “LOW-NORMAL-HIGH”.
On the other hand, even if the units to be entered in the setting item column do not match between the models or versions, the same unit may be entered on the setting screen. For example, in FIG. 4, the unit of the sampling interval is a specification that can be set in hertz (Hz), but in an actual apparatus, the specification is set in milliseconds (msec). On the setting screen 40, the unit can be input in hertz (Hz) so as to be unified with other models / versions. When the setting is actually reflected on each device, unit conversion is performed.
By unifying the setting input format in this way, even if the model and version are different, the operator can make settings with little awareness of the difference in specifications.
Note that the unit conversion is performed after the control program 16 converts the unit of the setting information stored in the temporary area afterwards to set each device.

  Also, by selecting a tab, other devices can be switched to input. For example, in FIG. 4, when setting the pump, the tab of 42b, the tab of 42c when setting the autosampler, the tab of 42d when setting the column oven, the tab of 42e when setting the UV detector, When setting the FL detector, the setting item column of each device is displayed on the setting screen 40 by selecting the tab 42f. Thus, it is not necessary to switch the setting screen one by one when setting each device, so that the burden on the operator is reduced.

The operation of the control program 16 will be described. The control program 16 reflects the setting information of each device input to the setting screen 40 on each device. When reflecting the setting information, after referring to the temporary area 14, the setting file in each device may be directly rewritten, or the setting screen displayed on each device is launched and the user interface of each device is used. May be set.
A specific example of a setting screen for a single PDA detector is shown in FIG.
4 and 5 are different in the order of the setting items. This is because the order of the setting item fields in FIG. 5 is changed by the user interface display mechanism 18 in order to unify the display of FIG. 4 with other models. This is because the setting screen 40 is displayed.
When the information input in the setting item field of FIG. 4 is reflected on the setting screen of the actual device of FIG. 5, the control program 16 operates to operate the keyboard by using a shortcut, etc. You may decide to change and set. That is, an appropriate setting value is input at an appropriate position while switching the setting item column by a tab operation.

  In addition, when inputting directly to the setting file of each device, the contents are rewritten to conform to the storage format of the setting file of each device. For example, if the setting values of a device are saved in a format that separates the setting values with “comma (,)”, the control program 16 creates the setting file by arranging the order of the setting values and then separating them with commas. Then, the setting file of the device is updated.

As described above, the chromatographic integration program 10 provides the temporary area 14 separately from the setting file of each device, and the information recorded in the temporary area 14 according to the setting method of each device by the control program is set for each device. It was decided to reflect on. As a result, even if the configuration screen of each device is unique, the display format can be generally unified, and the operator can set without being aware of the difference in model / version. Thereby, a sense of unity can be given to the operational feeling, and the work burden on the operator is reduced.
Also, setting items can be switched when inputting other devices by selecting a tab, and there is no need to switch the setting screen for each device.

As described above, the setting input of each device is integrated to facilitate input and reduce the burden on the operator.
However, other devices may start operating at the timing when one device starts or ends, and in this case, setting of the latter device becomes complicated. Based on the start or end timing of the operation of the former device, the operation of the latter device must be started at the same time or after a certain period of time, and the operator considers that This is because the start timing of the operation of the device must be set.
Therefore, a setting item related to the operation timing between the devices is provided in the setting item column displayed by the integrated program according to the present invention. As an example, if a new setting item called “response time” is provided, it is possible to start the operation of another device after the “response time” has elapsed since a certain device started or ended some operation. Become. This eliminates the need to consider the operation timing of the former device and facilitates the setting of the latter device.
For example, there is a case where the measurement wavelength of the UV (ultraviolet) detector is changed 3.0 seconds after switching the switching valve on the chromatograph. Normally, the UV detector is set in consideration of the switching timing of the switching valve so that the measurement wavelength of the UV detector is changed after 3.0 seconds from the switching timing of the switching valve.
However, in the present invention, since the setting item of “response time” is provided in the chromatograph integration program 10, it is not necessary to consider this when setting the UV detector, and the setting becomes easy. By setting the “response time” of the UV detector to 3.0 seconds, the measurement wavelength of the UV detector is changed after 3.0 seconds after the switching valve is switched.
In this way, the operation timing of each device is integrated and controlled, which greatly contributes to reducing the burden at the time of setting by the operator.

Next, output data integration will be described. FIG. 6 shows a schematic configuration of a high performance liquid chromatograph according to an embodiment of the present invention. The high-performance liquid chromatograph 60 shown in the figure includes a liquid feeding means 62 for feeding a mobile phase solvent, a sample injection means 66 for injecting a sample, a separating means 70 for separating a mixture, and a separating means 70. A detector (1) 74, a detector (2) 76 for detecting the separated components, and a computer 80 are provided. The detector (1) 74 and the detector (2) 76 can be provided with different types of detectors. In this embodiment, the detector (1) is a PDA detector and the detector (2) is fluorescent ( FL) detector.
The computer 80 includes main processing means 90, storage means 92, input / output control means 86, display means 82, and input means 88.

  What is characteristic in the present embodiment is that the high-performance liquid chromatograph program 94 unifies the user interface 84 that is an input screen and an output screen of information regarding each device of the high-speed liquid chromatograph 60 among the devices. This is realized by the computer 80. A high-speed liquid chromatograph program 94 is stored in the storage unit 92.

  As a result, in this embodiment, the input / output control means 86 of the computer 80 displays the liquid feeding means 62, the sample injection means (autosampler) 66, the separation means 70, and the detector (1) 74 on the screen of the display means 82. , And a user interface 84 that is an input screen and an output screen for information on the detector (2) 76.

  In the present embodiment, the user interface 84 unifies information input screens related to operation control of the detector (1) 74 and the detector (2) 76. Moreover, the user interface 84 unifies the output screen of the measurement data obtained by the detector (1) 74 and the detector (2) 76.

In the present embodiment, when the computer 80 executes the data display function of the high-performance liquid chromatograph program 94, a data display screen is displayed on the display means 82. One data display screen includes the detector (1) 74 and The measurement data obtained by the detector (2) 76 is displayed.
In the present embodiment, when the computer 80 executes the analysis result display function of the high performance liquid chromatograph program 94, an analysis result display screen is displayed on the display means 82, and one analysis result display screen includes a detector. (1) An analysis result based on the measurement data obtained by 74 and the detector (2) 76 is displayed.

The computer 80 also communicates from the detector (1) 74 and the detector (2) 76 and from each device other than the detector, such as the liquid feeding means 62, the sample injection means 66, the separation means 70, and the ultraviolet light. By integrating the communication from the visible detector 76 and displaying it on the user interface 84, it is displayed as one piece of information on the program. In the present embodiment, a two-dimensional chromatogram and a three-dimensional chromatogram obtained from the same sample are displayed with a sense of unity by a user interface 84 that unifies the appearance among the devices.
Further, the computer 80 integrates the signal from the detector (1) 74 and the signal from the detector (2) 76 obtained by measuring the same sample, and stores it as one data set 96 as a storage means 92. To save.

In the present embodiment, the liquid feeding means 62 includes a liquid feeding pump 64.
The sample injection means 66 is an autosampler and automatically injects the sample into the mobile phase sent from the liquid feeding means 62.
The separation means 70 includes a separation column 72 and a column oven 68. The column oven 68 includes a column 72.
The detector 74 (1) and the detector (2) 76 are connected in series to the outlet of the separation column 72.

In the present embodiment, the main processing means 90 includes a CPU and a ROM.
The storage unit 92 includes a hard disk.
The display means 82 includes a display and a printer.
The input means 88 includes a keyboard and a mouse.

The main processing means 90 is connected to the storage means 92 and to the display means 82 and the input means 88 via the input / output control means 86.
The main processing means 90 receives the three-dimensional data output from the detector (1) 74 (PDA detector), and receives the two-dimensional data output from the detector (2) 76. A data processing function for analyzing these data and a function for controlling the operation of each device 62, 66, 70, 74, 76 are combined. These functions are achieved by realizing various programs incorporated in the main processing means 90.

The high performance liquid chromatograph 60 according to the present embodiment is configured as described above, and its operation will be described below.
That is, in the present embodiment, in order to integrate the operation control and data collection of each device constituting the high performance liquid chromatograph 60, the appearance of the user interface 84 displayed on the screen of the display means 82 is detected by the detector ( 1) It is unified among 74, detector (2) 76, and each device 62, 66, 70 other than each detector.

As a result, in this embodiment, the unified user interface 84 can display the two-dimensional chromatogram and the three-dimensional chromatogram obtained from the same sample with a sense of unity.
In the present embodiment, communication from the detector (1) 74 and detector (2) 76 and communication from the devices 62, 66, and 70 other than the detector are integrated, and a high-performance liquid chromatograph program 94 is integrated. Can look like a piece of information.
In the present embodiment, the signal from the detector 74 (1) and the signal from the detector (2) 76 can be integrated and stored in the storage unit 92 as one data set 96.

  As a result, in this embodiment, the analyst is given a sense of unity with respect to operability, and the high-performance liquid chromatograph 60 including the detector (1) 74 is strongly conscious that one (the same) system is used. , Dispelling the unnaturalness felt by analysts and making the data uniform.

Conventionally, in order to integrate the operation control and data collection of each device constituting the high-performance liquid chromatograph, it has been a common means to unify hardware such as transfer means and communication means. In the embodiment, the appearance of the user interface 84 which is an information input screen and a display screen regarding each device constituting the high performance liquid chromatograph is unified among the devices.
As a result, in this embodiment, the conventional method, that is, the method of unifying the hardware such as the transfer means, is extremely difficult, and further improves the operation control and data collection of each device constituting the high-speed liquid chromatograph. Can be planned.

Hereinafter, the operation of the present embodiment will be specifically described.
<Communication>
After inputting the information, communication of information from the user interface 84 to each device is started.
In the present embodiment, the computer 80 integrates communication between the detector (1) 74 and the detector (2) 76 and other chromatograph-related devices. It can look like information.

<Measurement>
The mobile phase is caused to flow through the separation column 72 at a constant flow rate by the liquid feed pump 64, and the sample liquid is injected into the mobile phase from the autosampler 66 and sent to the separation column 72. While the injected sample passes through the separation column 72, the components in the sample are separated with different retention times.

<Data collection from each detector>
The eluted component from the separation column 72 is detected by the detector (1) 74 and the detector (2) 76, and a chromatogram is obtained.
Here, the detector (1) 74 is a PDA detector, which detects each component eluted from the separation column 72 by dispersing it in the wavelength direction at predetermined time intervals. This detection signal is sent to the main processing means 90. Data obtained by the detector (1) 74 is three-dimensional data including time, intensity, and wavelength.
The detector (2) 76 is a fluorescence detector, and detects a chromatogram of the fluorescence wavelength at predetermined time intervals. This detection signal is sent to the main processing means 90. Data obtained by the fluorescence detector 76 is two-dimensional data including time and intensity.

Here, in this embodiment, the computer 80 collects measurement data from the detector (1) 74 and collects measurement data from the detector (2) 76.
Therefore, in this embodiment, the computer 80 stores the signal from the detector (1) 74 and the signal from the detector (2) 76 in the storage unit 92 as one data set 96. Yes.
As a result, in this embodiment, the measurement data obtained by the detector (1) 74 and the detector (2) 76 can have a sense of unity.

<Analysis and information display>
After collecting the data, analysis is performed, and the analysis result is displayed on the screen of the display means 82.
Here, in this embodiment, the computer 80 adjusts the time series of the two-dimensional chromatogram and the three-dimensional chromatogram obtained from the same sample by the unified user interface 84 to give a sense of unity, and the analysis result Is displayed.
As a result, in this embodiment, the analyst is given a sense of unity with respect to operability, the high-performance liquid chromatograph 60 including the detector (1) 74 is strongly conscious of being used in the same system, and the analyst It is possible to remove the unnatural feeling and to make the data uniform.

Hereinafter, the operation of the present embodiment will be described more specifically.
In the present embodiment, the user interface 84 includes a device configuration setting screen, a condition setting screen, a data display screen, and an analysis result display screen that are common to each device. The high performance liquid chromatograph program 94 according to the present embodiment includes an apparatus configuration setting function, a condition setting function, a data display function, and an analysis result display function.

(Monitor during data collection)
If a plurality of detectors are connected, a plurality of chromatograms are output. Some output a plurality of two-dimensional chromatograms from a single detector. In order to distinguish them, data channels are usually attached with numbers, alphabets, and the like.
As shown in FIGS. 7 and 8, in this embodiment, a two-dimensional chromatogram is output by two methods. One is a two-dimensional chromatogram collected from each detector except the PDA detector. This is hereinafter referred to as a (direct) measured two-dimensional chromatogram 102. The other is a two-dimensional chromatogram extracted by selecting a specific wavelength from the three-dimensional data (three-dimensional chromatogram 104) obtained by the PDA detector. This is hereinafter referred to as a two-dimensional chromatogram 105 extracted (from PDA data).

Further, with respect to the method of displaying the entire three-dimensional chromatogram 104, a contour display (for example, the X axis (elapsed time) in the horizontal direction of the screen, the Y axis (wavelength) in the vertical direction, and the intensity is displayed by color) 106) and a 3D display that draws a cube on the screen and plots the X axis (elapsed time), the Y axis (wavelength), and the Z axis (intensity).
Up to now, the measured two-dimensional chromatogram output from the detector (2) 76, etc. in FIG. 6 is displayed on the program screen dedicated to each detector, and from the PDA detector of the detector (1) 74 in FIG. The extracted two-dimensional chromatogram and three-dimensional chromatogram were displayed on the screen of the dedicated program. In this embodiment, what is separately displayed in this way is stored on one screen.

  In the present embodiment, the user interface 84 includes a data display screen common to each device. By only instructing execution of one data display function, one data display screen is opened. On one data display screen, the measurement data obtained by the detector (1) 74 and the measurement data obtained by the detector (2) 76 are displayed.

  In the present embodiment, the measurement data display screen obtained by the detector (1) 74 and the measurement data display screen obtained by the detector (2) 76 are opened by different operations. Compared with the case where the measurement data obtained by the detector (1) 74 and the measurement data obtained by the detector (2) 76 are displayed on a separate screen (separate window), the appearance and the unified feeling of operation are improved. It is illustrated.

  For example, as shown in FIG. 7, a data collection time data display screen 100, which is an example of a user interface, is displayed on the screen of the display means, and the measured two-dimensional chromatogram 102 is extracted from the top of the screen. By arranging the contour display 106 of the two-dimensional chromatogram 105 and the three-dimensional chromatogram 104 (FIG. 8) in the vertical direction, the impression that all the data measured from one analysis system is being monitored at a time. It can be strongly given to analysts.

Here, the measured two-dimensional chromatogram, the extracted two-dimensional chromatogram, and the three-dimensional chromatogram may have different data point intervals (data acquisition intervals). For this reason, when the display of each chromatogram is arranged in the vertical direction, it is assumed that the length of chromatograms will shift. Therefore, as shown in the figure, by aligning the scales of the X axis (elapsed time, horizontal axis) in each data, for example, the measured chromatogram 102, the extracted chromatogram 105, and the contour display 106 of the three-dimensional chromatogram. It becomes possible to give a sense of unity more.
In the present embodiment, the design is unified by unifying the color usage, font, and drawing method.

(Data collection integration)
In the present embodiment, when collecting data, the computer 80 also uses the three-dimensional chromatogram 105 obtained from the detector (1) 74 and the measured two obtained from the detector (2) 76 as shown in FIG. The two-dimensional chromatogram 102 is handled as one aggregate by the high-performance liquid chromatograph program 94.

(Data storage output from each detector)
Furthermore, in this embodiment, the two-dimensional chromatogram 105 extracted from the three-dimensional chromatogram 104 collected as described above is extracted, and all of these chromatograms 102, 104, and 105 are obtained from one sample. Treated as a measurement data set 96.
This data set 96 is centrally managed and stored in a storage means 92 such as a hard disk or a database.

(Data analysis)
In the present embodiment, the user interface includes an analysis result display screen common to each detector. The analysis result display screen is opened simply by instructing the execution of one analysis result function. On one analysis result display screen, an analysis result based on measurement data obtained by the PDA detector (detector (1)) and a detector other than the PDA detector (detector (2), etc.) were obtained. The analysis result based on the measurement data is displayed.
In the present embodiment, the display screen of the analysis result based on the measurement data obtained by the PDA detector and the analysis result display screen based on the measurement data obtained by another detector are opened by different operations. Compare the analysis result based on the measurement data obtained by the PDA detector and the analysis result based on the measurement data obtained by other detectors with those displayed on a separate screen (in a separate window) A sense of unity is improved.

Also, when the analyst opens the data, it is identified by the measurement data set obtained by each analysis, so the measured two-dimensional chromatogram, extracted two-dimensional chromatogram, three-dimensional chromatogram obtained by one analysis Can be handled collectively. That is, in this embodiment, programs for analyzing measured data are also collected on one screen.
A screen for displaying stored data, that is, a stored data display screen as an example of the user interface of the present embodiment is also measured from the upper part of the screen as shown in FIG. If the extracted two-dimensional chromatogram 105 and the contour display 106 of the three-dimensional chromatogram are arranged vertically and the scales of the X-axis (elapsed time) are aligned, all the data measured from one analysis system can be obtained. You can see at a glance. If cursors that move in synchronization are displayed on all the chromatograms arranged in the vertical direction, the positions of the peaks can be directly compared.
The mouse operation, menu operation, button operation, and key operation are unified, and the menu and tool buttons are integrated to further increase the sense of unity.
As for peak detection, the intensity and shape of the entire chromatogram generally differ for different channels. For this reason, it may not be very likely that different channels can be processed with the same peak detection parameters, but all channels are not used during peak periods (from injection to elution time of non-retained components). Is almost equal. For this reason, if there is not much difference in the intensity of the chromatogram of each channel, the peak detection parameter can be shared, which is convenient.
Furthermore, on the analysis result display screen 84d (user interface) as shown in FIG. 9, the quantitative value is calculated by peak detection, identification, and calibration curve, and the calculation result of the same component (peak) is calculated. The grams 102a and 102b and the extracted chromatograms 105a and 105b can be combined and displayed for each channel. The methods for peak identification and calibration curve creation (quantitative calculation) in this case are unified so that both the measured two-dimensional chromatogram and the extracted two-dimensional chromatogram can be handled.
The printed report also allows you to print the measured 2D chromatogram, the extracted 2D chromatogram, and the 3D chromatogram on the same sheet, and see a list of measurement data obtained from one sample. So that it can be taken.

As described above, in the conventional method, for example, as shown in FIG. 10A, the user compares the three screens 120, 122, and 124, but in the present embodiment, the same figure (B). As shown in FIG. 4, the user switches the contents 84e, 84f, 84g of one screen (user interface).
As a result, this embodiment gives the analyst a sense of unity with respect to operability compared to the conventional method, and makes a high-performance liquid chromatograph including a plurality of detectors strongly aware that one system is used, It is possible to eliminate unnaturalness felt by analysts and to make data uniform.

Further integration In this embodiment, in order to further integrate the PDA detector of the high-performance liquid chromatograph with other detectors, the detector connection position and chromatogram output as described below. It is very preferable to consider the order and the scale adjustment at the time of chromatogram output.

(1) Detector connection position In this embodiment, in order to integrate the PDA detector connected in series behind the column unit with other detectors, the same peak depending on the detector connection position is used. It is also very important to correct the holding time shift.
That is, in general, when the measured two-dimensional chromatogram and the extracted two-dimensional chromatogram are displayed side by side in the vertical direction on the screen of the display means, there may be a deviation in the detection peak retention time. The retention time here means the time taken from the sample introduction point to the peak peak.
This is because each two-dimensional chromatogram is based on measurement data from different detectors, and these detectors are connected in series behind the column unit. Therefore, it is because a flow path difference arises between each detector. The components (peaks) separated by the column unit are discharged from the column unit and then pass through the detectors connected in series. At this time, the time for passing the detector in the subsequent stage is usually delayed as compared with the time for passing the detector in the previous stage.

On the other hand, in this embodiment, the computer measures a sample including a component that can be an index of the retention time such as an internal standard in advance in order to perform the identification by correcting the shift of the retention time of the peak at each detector. Then, a peak identification table 98 (FIG. 6) is created. That is, the computer corrects the shift in the retention time of each detector of the same component based on the retention time of the standard substance.
The computer compares the retention time on the chromatograph obtained by the PDA detector with the retention time on the chromatograph obtained by another detector based on the retention time of the standard substance, and detects each detection. Find the difference in holding time between vessels.
That is, in the present embodiment, the mobile phase solvent is allowed to flow by the liquid feeding means, and the internal standard substance that can be detected at all the extracted measurement wavelengths of all the detectors of the high performance liquid chromatograph and the PDA detector, etc. Control the operation of each device so that a sample containing a component that can be an indicator of retention time is injected from the sample injection means, the internal standard substance from the separation means is detected by each detector, and the data of each detector is collected. , Let the computer run.
Here, the computer detects the peak apex corresponding to the internal standard substance from the chromatogram obtained based on the data of each detector, and automatically calculates the delay time between the detectors.
The computer controls each device and collects data based on the obtained delay time between the detectors. For example, the computer manages the peak identification time at each detector.

In this embodiment, when setting the identification time of the same component to each detector, the computer inputs another holding time (identification time) detected by the most connected detector so that the computer can detect other detectors ( Channel) is automatically obtained by correcting the identification time with the calculated delay time.
As a result, in this embodiment, the identification time at the other detector can be controlled by the computer on the basis of the holding time (identification time) detected by the most connected detector.
Therefore, in the present embodiment, the overall control of the control of each detector and the overall management of data collection can be more reliably realized by the computer.

(2) Order of output of chromatograms In this embodiment, in order to further integrate the PDA detector and other detectors, the computer displays the chromatogram obtained by each detector on the screen of the display means. It is very preferable to arrange the chromatograms in the order in which the detectors are connected when the grams are output in the vertical direction.
For example, as shown in FIG. 11A, when a PDA detector 74, a fluorescence detector (FL) 76b, and a differential refractive index detector (RI) 76c are connected in series after the separation column 72, As shown in FIG. 5B, the computer performs two-dimensional chromatogram 105a of PDA 220 nm, two-dimensional chromatogram 105b of PDA 280 nm, two-dimensional chromatogram 102a of fluorescence detector (FL), differential refractive index detector (RI). ) Are arranged in the vertical direction on the screen of the display means and output.

As described above, in the present embodiment, when the computer arranges the chromatograms in the vertical direction and displays them on the screen, the computer arranges the chromatograms in the order of connection of the target detectors instead of the channel numbers. The delay time between the detectors can be calculated. In order to calculate the delay time, the measurement sample includes an internal standard that can be detected by all detectors (and all extracted measurement wavelengths), and the computer automatically calculates the delay time between each detector. Is preferred.
For example, as shown in FIG. (B), the deviation time a between retention time in the retention time and fluorescence detector at PDA detector from the position of the elution peak P ₁ (FL), for example, held in the PDA detector A deviation time b between the time and the holding time in the differential refractive index detector (RI) can be obtained. Also, the position of the elution peak P _2, it is possible to obtain the deviation time c the retention time in the fluorescence detector retention time and a differential refractive index detector at (FL) (RI).

  The advantage of this is that when creating the peak identification table, when entering the identification time of the same component (peak) detected in all channels or multiple channels, the most forward connection is made for the target component (target peak). By inputting only the holding time (identification time) detected by the detected detector (PDA), the computer automatically corrects the identification time of other detectors (channels) with the calculated delay time. Can be asked.

For example, in the peak identification table as shown in FIG. 5C, only the holding time (identification time) detected by the detector connected to the foremost part is input for the target component (target peak).
In the figure, only the retention time (identification time) = 2.000 detected by the PDA is input for peak 1. In the figure, only the retention time (identification time) detected at FL = 5.000 is input for peak 2.

As a result, the identification time of each peak at each detector is as follows.
The identification time at the peak 1 FL detector is 2.000 + a
The identification time at the peak 1 RI detector is 2.000 + b
The identification time at the RI detector for peak 2 is 5.000 + c

(3) Scale adjustment In the present embodiment, in order to further integrate the PDA detector and other detectors, it is also very preferable to adjust the scale when outputting the chromatogram.
That is, the data acquisition interval may differ between the measured two-dimensional chromatogram, the extracted two-dimensional chromatogram, and the three-dimensional chromatogram. When chromatograms with different data acquisition intervals are arranged in the vertical direction, the number of data points is different, and therefore the scale in the X-axis (elapsed time) direction cannot be adjusted. If the scales cannot be adjusted, even if they are arranged vertically, the scales are scattered and there is no point in arranging them.

  On the other hand, in the present embodiment, the computer includes a data storage function and a scale adjustment function for adjusting the scale.

(I) Data to be stored In this embodiment, the computer stores the measurement data from each detector in a storage unit in a table including at least one common data item.
In this embodiment, for example, as shown in FIG. 12A, each chromatogram data from channels A and B has a retention time (elapsed time) as a common item, and a data point ID and a retention time (elapsed time). ), Data of three items of intensity are stored in a table.

(Ii) Scale adjustment In this embodiment, since the computer provides a sense of unity between the information display screen related to the photodiode array detector and the information display screen related to other detectors based on the data of the common items, Each detector data stored in the means is displayed on the screen of the display means.
In the present embodiment, for example, as shown in FIG. 5B, when the computer displays the chromatograms in the vertical direction on the screen, the scales of the X-axis (elapsed time) of the chromatograms coincide with each other. Thus, the scale of the X axis (elapsed time) of each chromatogram is adjusted.
In this way, the computer can appropriately and easily compare the chromatograms by arranging the chromatograms on the screen in the vertical direction and displaying them on the screen.
As described above, in this embodiment, the computer can correlate the data at the time of storage and display based on the data of the retention time (elapsed time) which is an item common between the detectors. It is possible to reliably integrate the collection.

<Type of detector>
In the present embodiment, a mass spectrometry detector (MS) can be handled in the same manner as the photodiode array detector (PDA).

DESCRIPTION OF SYMBOLS 10 Chromatograph integrated program 12 Setting screen 14 Temporary area 16 Control program 18 Model / version discrimination mechanism 19 User interface display mechanism 20 Control computer 30 Model / version display screen 32 Connection status display box 34 Device type name display column 36 Device name display Column 40 Setting screen 42a PDA detector setting tab 42b Pump setting tab 42c Autosampler setting tab 42d Column oven setting tab 42e UV detector setting tab 42f FL detector setting tab 50 PDA detector setting screen used in this embodiment 60 High-performance liquid chromatograph 62 Liquid feed means 64 Liquid feed pump 66 Sample injection means 68 Column oven 70 Separation means 72 Separation column 74 PDA detector 76 Detector other than PDA detector 80 Computer 82 Display means 8 User interface 86 Input / output control means 88 Input means 90 Main processing means 92 Storage means 94 High-speed liquid chromatograph program 96 Data set 98 Identification table 100 Data display screen 102 during data collection Measured two-dimensional chromatogram 104 Three-dimensional chromatogram 105 Extracted two-dimensional chromatogram 106 Contour display 110 SCSI
112 RS232
120 Device control monitor screen 122 HPLC data measurement analysis screen 124 PDA detector measurement analysis screen

Claims (9)

In an integrated program that integrates chromatograph-related instruments having independent control programs and configuration files,
Chromatographic equipment
A column unit that separates substances into components using the difference in physical properties of substances contained in the sample;
Two or more detectors connected to the rear of the column unit,
Each chromatograph-related device is connected to the control computer via the communication interface of each standard,
It comprises an output integration mechanism for converting the output information of each detector into a desired unit, unifying the time axis scale, and displaying two or more two-dimensional chromatograms or three-dimensional chromatograms in parallel. Chromatograph integration program. The program according to claim 1,
A chromatograph integration program, wherein a two-dimensional chromatograph having a specific wavelength is extracted from the three-dimensional chromatogram. In the program according to claim 1 or 2,
The two or more detectors are connected in series behind the column unit,
The output integration mechanism corrects a detection delay due to a flow path difference between a front-stage detector and a rear-stage detector connected in series. In the program according to claims 1 to 3,
The integrated program includes a user interface display mechanism for displaying a user interface for collectively displaying setting items of each device in one setting item column;
A model that determines the model / version of each device by connecting the two or more devices to the control computer, selects the setting items necessary for each device, and provides information related to the setting items to the user interface display mechanism A chromatograph integration program further comprising a version discrimination mechanism. The program according to claim 4, wherein
The integrated program allows the setting of each device to be input in the desired unit on the user interface by the control program even when the model / version of each device is different, and corresponds to the setting items of each device A chromatograph integration program, further comprising: a setting unit integration mechanism that performs unit conversion by converting the input information to make the settings of each device. In the program according to claims 1 to 5,
A setting item displayed as a user interface by the user interface display mechanism is further provided with a setting item relating to operation timing control between the chromatograph-related devices, and the operation of a device is set by setting the operation timing of the interlocking device. The setting related to the operation timing of the other device according to the information input to the setting item related to the control of the operation timing based on the timing at which the operation of the device starts or ends so that the other device responds appropriately An integrated chromatograph program characterized by In the program according to claim 4-6,
The integrated program starts a setting program for each detector, starts up a user interface of each chromatograph-related device, and sets each detector by inputting setting information on the user interface. Chromatograph integration program. In the program according to claim 4-7,
The integrated program is a chromatographic integrated program characterized in that each detector is set by directly rewriting a setting file of each detector. In the chromatograph integration program according to claim 4-6,
The integrated program performs the same operation as the keyboard operation on the setting screen of each device, inputs the setting value in the setting item field of each device, and sets each device. Graph integration program.

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