JP7608570B2 - Autosampler control device and automatic measurement system including same - Google Patents

Description

The present invention relates to a control device for an autosampler installed in a measuring device such as a chromatograph device, and an automatic measurement system including the same.

Conventionally, in measurements using liquid chromatography (HPLC) devices and the like, an autosampler is used to automate the introduction of samples into the device. This autosampler includes a sample holder, such as a rack, that holds a number of samples in an array, and a sample introduction section that introduces the samples one by one into the measurement device. Here, for example, sequence numbers are assigned to indicate the order in which the samples are introduced from the sample holder.
Conventionally, the measurement order (introduction order) of samples using an autosampler is set by inputting the sample position, measurement conditions, etc. for each sequence number of the sample holder in a reservation table on the screen of the device.
However, inputting data in a table format requires complicated operations, and it is difficult to intuitively grasp the actual placement position of the sample on the sample holder when inputting data in a table, which makes it prone to input errors.
In response to this, a technology has been developed that displays the arrangement of samples in the sample holder on a screen, allowing the measurement order and measurement conditions of the samples to be set in tabular form while checking the display screen (Patent Document 1).

Patent No. 3394744

12, in the method described in Patent Document 1, a window for an analysis reservation input table 500 and a window for a sample holding diagram 600 showing the actual arrangement (holding) state of samples are displayed on the display screen. In this case, the sample at position 2-2 (2nd column, 2nd row) of the sample holder with sequence number 1 is measured first, followed by measurements of samples at positions 1-1 (1st column, 1st row) and 4-2 (4th column, 2nd row) of the sample holder with sequence numbers 2 and 3, respectively.
However, if the order of the samples on the sample holding diagram 600 differs from the order of the samples measured based on the sequence number, it is difficult to know where the next sample to be measured is located, which causes a problem that it is difficult to make changes, such as replacing a sample that has a defect before starting the next measurement, or urgently measuring another sample.
Furthermore, when changing the measurement order, the user must return to the analysis reservation input table 500 and input the position of the sample that is to be measured first, which is cumbersome and prone to errors.
In particular, in the case of blood tests in hospitals, etc., there are many non-routine tasks such as tests on emergency patients being interrupted, making the above-mentioned problems more likely to occur. In addition, mistakes such as mixing up samples can become a serious problem.

Therefore, the present invention has been made to solve the above-mentioned problems, and aims to provide an autosampler control device and an automatic measurement system including the same, which can easily determine the position of the next sample to be measured based on holding position information that indicates the actual holding position of the sample.

In order to achieve the above-mentioned object, the autosampler control device of the present invention is used in an autosampler equipped with a sample holding section that holds multiple samples in an array and a sample introduction section that introduces the multiple samples one by one into a measuring device, and is an autosampler control device having a control section and a memory section, wherein the control section displays holding position information indicating the holding positions of the multiple samples in the sample holding section on a specified display section, the holding position information having a sequence number that is the arrangement order of the samples in the sample holding section and measurement selection information indicating whether or not a measurement reservation is made, and when the measurement selection information indicates a state where a measurement reservation is made at the time the current measurement is completed, the control section controls the sample introduction section to introduce the samples for which the measurement selection information indicates a state where a measurement reservation is made into the measuring device in order of the sequence numbers, starting from the earliest .

According to the control device of this autosampler, it is easy to know the position of the next sample to be measured based on the holding position information indicating the holding positions reflecting the actual arrangement order (measurement order) of each sample .

In the control device of the autosampler of the present invention, the control unit may transmit to the measuring device measurement conditions corresponding to the type of sample for which the measurement selection information indicates that a measurement reservation has been made and which will be next introduced into the measuring device in the order of the sequence numbers .

In the autosampler control device of the present invention, when the sample is selected by a user on the holding position information, the control unit may display corresponding information regarding the sample .

The automatic measurement system of the present invention includes a control device for the autosampler, the autosampler, and the measurement device.

The automated measurement system of the present invention may be a liquid chromatographic measurement system.

The present invention provides an autosampler control device that can easily set and change the measurement state of a sample based on holding position information that indicates the actual holding position of the sample, and can easily grasp the measurement state.

1 is a diagram showing a configuration of an automatic measurement system (liquid chromatograph apparatus) according to an embodiment of the present invention. FIG. 2 is a diagram showing the configuration of an autosampler. FIG. 11 is a diagram showing holding position information displayed on a display unit. FIG. 13 is a diagram showing a case where one of the measurement statuses of a predetermined sample is specified by a user on the holding position information. FIG. 13 is a diagram showing an information setting window that prompts the user to set the type of sample when the information setting status is specified by the user. FIG. 13 is a diagram showing a case where a user specifies a measurement reservation status. FIG. 13 is a diagram showing a case where a user cancels the measurement reservation status. FIG. 4 is a diagram illustrating a table stored in a storage unit. FIG. 13 is a diagram showing a case where a measurement result is displayed when a user selects a specific sample on the holding position information. FIG. 13 is a diagram showing another example of the sample holder and holding position information representing the same. 3 is a schematic diagram showing a diluted sample for creating a calibration curve held in a sample holding section and a dilution container; FIG. FIG. 1 is a diagram showing a method for specifying the measurement order of samples in a conventional autosampler.

Hereinafter, an embodiment of the present invention will be described with reference to the drawings.
FIG. 1 is a diagram showing the configuration of an automatic measurement system (liquid chromatograph apparatus) 100 according to an embodiment of the present invention.
The liquid chromatograph apparatus 100 performs qualitative or quantitative analysis of a specified measurement target, and is equipped with a data processing device (control unit) 7 that controls the entire system, a mobile phase (a mixed solution of eluent and solvent) 1, a pump 2 that delivers the mobile phase 1, an autosampler 3 that injects samples, a column 4 that separates components, a column oven 5 that keeps the column 4 at a constant temperature, a detector 6 that detects the separated components, and a display unit 10.
The data processing device 7 is composed of a computer having a control unit (CPU) 9 that executes the analysis and analyzes the analysis results, and a storage unit (hard disk, etc.) 8 that stores the analysis results. The display unit (monitor) 10 displays the analysis results and is a touch panel, allowing the user U to perform various inputs, selections, settings, etc. on the display unit 10 instead of a keyboard, etc.

The detector 6 corresponds to the "measurement device" in the claims. The data processing device 7 corresponds to the "autosampler control device" in the claims. In other words, the autosampler control device according to the embodiment of the present invention can be retrofitted and applied to any measurement device.
Moreover, the liquid chromatograph 100 corresponds to the "automatic measurement system" in the claims.

The detector 6 has an element for detecting the signal intensity, and detects the signal intensity with respect to time. As the detector, a three-dimensional detector having a plurality of detection elements and capable of simultaneously acquiring signals at a plurality of wavelengths can also be used.
A sample is injected from an injector (not shown) of an autosampler 3, passes through a column 4 together with a mobile phase 1 delivered by a pump 2, and is separated into various components in the sample.
The sample separated into its components is detected by a detector 6. A signal from the detector 6 is sent to a data processing device 7 where data processing is performed.
The column 4 is a device generally used as a separation section for separating components of a sample present in the mobile phase 1. Examples of the column 4 include a packed column and a monolith column. Various types of column packing materials can be used for the column 4, such as an adsorption type, a distribution type, and an ion exchange type. The column 4 is desirably placed in a column oven 5 so that the column 4 can be kept at a constant temperature and the sample can be separated with good reproducibility.

The memory unit 8 stores measurement conditions for each type of sample, calibration curve data, etc. As shown in FIG. 8, the memory unit 8 also stores the measurement status and sample type in table 8t for each of the following sample holding positions (sequence numbers).

As shown in FIG. 2, the autosampler 3 includes a sample holder 3a that holds a plurality of samples (vials) 201a, 201b in an array, and a sample introduction section 3b that introduces the plurality of samples one by one into the measuring device.
Here, the sample holding portion 3a is a holder having ten holding holes 3h in a row for holding samples 201a, 201b, ..., and the holding holes 3h are arranged in a sequence such that measurements are taken in order from the left side of Figure 2.
The sample introduction section 3b includes an arm 3t, a needle-equipped head 3s that is mounted on the underside of the arm 3t and introduces multiple samples one by one into the measuring device (detector 6), and a moving mechanism (a well-known actuator, not shown) that moves the arm 3t in the planar and vertical directions.

In this example, the sample is a liquid, and is placed in a vial (container) and sealed with a top lid. The needle head 3s is inserted into the top lid of the vial, and the sample inside the vial is sucked up and introduced into the injector.
The sample may be a solid or powder. In this case, the sample is placed directly on a sample holder such as a turret, and then grasped by a gripper provided in the sample introduction section and transported to the measuring device.
Therefore, in the present invention, "introduction" includes cases where a sample, such as a liquid inside a container, is moved to a measurement site of a measuring device without moving the container held in the sample holding section, and cases where the sample is moved directly to the measurement site of a measuring device.
In addition, the measuring device may be, in addition to the detector 6, a fluorescent X-ray analyzer or the like, but is not limited to these.

Next, operations performed by the control unit 9 in response to operations performed by the user while looking at the display screen of the display unit 10 will be described with reference to FIGS.
FIG. 3 shows holding position information 300, which is displayed on the display unit 10 under the control of the control unit 9, and which indicates the holding positions of a plurality of samples in the sample holder 3a.
3, the autosampler 3 can be equipped with two sample holders 3a, each of which holds 10 samples (vials) arranged in a row, and the actual sample holders 3a corresponding to the upper row 300x of the holding position information 300 hold predetermined types of samples such as Blank, Std (standard material), etc. On the other hand, the actual sample holders 3a corresponding to the lower row 300y hold UNK (unknown samples), and some of the holding holes 3h among them do not contain samples (vials).

Taking the lower row 300y of the holding position information 300 as an example, the holding position 302 of each sample is displayed in a circle, and the consecutive order (sequence number) is displayed inside the circle. The order of measurement of the samples (order of introduction into the detector 6) is performed in ascending order of sequence numbers, and in this example, measurements are performed from 1 to 10 in the upper row 300x of the holding position information 300 from the left (blank) to the right, and then measurements are performed from 11 to 20 in the lower row 300y from the left to the right.
Furthermore, the type of sample (blank, CBZ, UNK, etc.) 306 is displayed above the holding position 302, and measurement selection information (check boxes) 304, which will be described later, is displayed below the holding position 302.

FIG. 4 shows a case where a user U specifies one of the measurement statuses of a specific sample (sequence number 15) on the holding position information 300.
The measurement status indicates one of a number of measurement states, and in this example, an unset status 310 (white circle for each sample in FIG. 4), an information setting status 312 (gray hatched circle for each sample in FIG. 4), and a measurement reservation status, a measuring status, and a measured status, which will be described later, are assigned.

The controller 9 automatically assigns the unset status 310, the measuring status, and the measured status even if the user U does not specify them.
The unset status 310 is a status in which no measurement status has been set, except for the measuring status and the measured status.
The fact that measurement is in progress can be recognized, for example, when the control unit 9 receives a signal indicating that measurement is in progress from the detector 6 after a sample designated by the measurement reservation status 314 is introduced into the detector 6 .
The fact that the measurement has been completed can be recognized by the control unit 9 receiving, for example, a signal indicating that the measurement has been completed (or data on the measurement result) from the detector 6 side.

In FIG. 4, for example, when user U clicks on sample (sequence number 15), the control unit displays the information setting window 312W in FIG. 5 on the display unit 10, superimposed on the holding position information 300.

In the input box 312Wa of the information setting window 312W in Fig. 5, the user U is prompted to set the type of sample, and inputs the type appropriately in the input box 312Wa, or if the type candidates have been determined in advance, selects the type using a selection bar or the like, and clicks the set button 312Wb to confirm the selection. In Fig. 5, carbamazepine (abbreviated as CBZ) is selected. The information setting status 312 is finalized only when the set button 312Wb is clicked.
As a result, the control unit 9 associates the sample position (sequence number 15), the information setting status 312, and the sample type (carbamazepine) with each other and stores them in the memory unit 8. The control unit 9 also displays the sample (sequence number 15) for which the information setting status 312 is specified in a color-coded manner or highlights it on the holding position information 300. In this example, the sample (sequence number 15) is displayed in a color-coded manner using gray hatching.
In this manner, in FIG. 4, three consecutive samples (sequence numbers 13 to 15) are displayed in different colors to indicate that they are in the information setting status 312.

As described above, in this embodiment, by selecting a sample on the holding position information 300 indicating the holding positions 302 that reflect the actual arrangement order (measurement order) of each sample, the measurement status of each sample can be visually and easily set and changed in correspondence with the arrangement order of the samples.
Furthermore, since the measurement status of each specified sample is displayed in a different color or highlighted, the arrangement order of the samples and their measurement status can be easily grasped visually.
As a result, it becomes easier to replace a sample before a measurement or to interrupt a measurement of another sample while checking the measurement status.

Next, the measurement reservation status will be described with reference to Fig. 6. In this example, the user U checks the measurement selection information (checkbox) 304 for the sample (sequence number 15) to specify the measurement reservation status 314.
The control unit 9 displays the sample (sequence number 15) for which the measurement reservation status 314 has been specified in a different color using diagonal hatching, and stores the sample position (sequence number 15) and the measurement reservation status 314 in association with each other in the memory unit 8.
In addition, when the current measurement (sample with sequence number 12) is completed, the control unit 9 controls the sample introduction unit 3b to introduce the samples (sequence numbers 13 and 15) specified by the measurement reservation status 314 into the detector 6.
As a result, the samples with sequence numbers 13 and 15 are measured in order.
In addition, when performing the measurement, the control unit 9 refers to the memory unit 8 and transmits the measurement conditions corresponding to the type (carbamazepine) of the sample to be measured (sequence number 15) to the detector 6, and the detector 6 performs the measurement according to those conditions.

Here, the sample currently being measured (sequence number 12) is automatically assigned a measuring status 316 and is displayed in a different color with horizontal hatching.
Moreover, a measured sample (sequence number 11) is automatically assigned a measured status 318 and is displayed in a different color using cross-hatching.

As shown in FIG. 6, when a user U specifies a measurement reservation status 314 for a sample (e.g., sequence number 19) for which an information setting status 312 is not specified (i.e., unset status 310), the control unit 9 invalidates the specification.
This makes it possible to prevent erroneous measurement of a sample whose type and other measurement conditions are not specified.

As shown in FIG. 6, if there are multiple samples (sequence numbers 13 and 15) for which the measurement reservation status 314 is specified, the control unit 9 introduces the samples into the detector 6 in the order of the sample corresponding to the earliest sequence number in a predetermined consecutive arrangement (sequence) of samples in the sample holder 3a. In other words, the measurements are performed in the order of sequence numbers 13, 15, etc.

On the other hand, as shown in Fig. 7, the user U can also cancel (cancel) the measurement reservation status 314 by unchecking the check box 304. In Fig. 7, the measurement reservation status 314 of the sample with sequence number 13 is cancelled, and the control unit 9 deletes the information on the position of the sample with sequence number 13 and the measurement reservation status from the storage unit 8, and terminates the color-coded or highlighted display of the sample as the measurement reservation status 314 of sequence number 13. When the check is removed, the status returns to the previous state display.
As a result, the measurement of the sample with sequence number 13 is stopped, and the measurement of the sample with sequence number 15, which is the next earliest sequence number, is performed.

As described above, in this embodiment, by using the measurement reservation status indicating the next measurement as the measurement status, the sample to be measured next can be visually and easily set and changed on the holding position information 300 that reflects the actual arrangement order (measurement order) of each sample. Furthermore, the position of the sample to be measured next can be easily grasped.
In addition, a measurement reservation status can be specified for multiple samples, and the measurement order will be the actual order in which the samples are arranged. This also makes it easy to know the position of the next sample to be measured, and since multiple samples can be scheduled for measurement, forgetting to measure them can be prevented.
Furthermore, since the measurement reservation status can be designated or cancelled by checking the measurement selection information (checkbox) 304, designation or cancellation can be easily and visually grasped.

Next, returning to FIG. 5, the measurement of the calibration curve will be described.
When the user U checks the calibration curve creation check button (calibration curve information) 312Wd in the information setting window 312W of FIG. 5, the control unit 9 automatically creates a calibration curve for the type of sample (carbamazepine) specified in the information setting window 312W.
First, as shown by the sample (sequence number 3) in the upper row 300x of the holding position information 300 in FIG. 4, a standard sample for creating a calibration curve corresponding to the type of sample (carbamazepine: CBZ) is held in advance at a predetermined position in the actual sample holding unit 3a, and the memory unit 8 stores in advance the position of this standard sample.
The control unit 9 refers to the memory unit 8 and controls the sample introduction unit 3b to introduce the CBZ standard sample with sequence number 3 from the actual sample holder 3a into the detector 6, and causes a calibration curve measurement to be performed.

In order to create a calibration curve, standard samples of multiple concentrations are required, but it may be difficult to hold multiple standard samples of each concentration in the sample holder in advance due to space limitations. Therefore, it is possible to prepare diluted standard samples of multiple concentrations from a standard sample of one concentration (the CBZ standard sample of sequence number 3) each time a calibration curve is created.
11 shows a diluted sample (dilution liquid) 201c for creating a calibration curve held in the sample holding section 3a, and an empty dilution container 201d. The diluted sample (vial) 201c contains a dilution liquid 201s. In FIG. 11, the diluted sample 201c and the empty container 201d correspond to sequence numbers 9 and 10 in FIG. 3, respectively.
Moreover, the memory unit 8 pre-stores the positions of the diluted sample 201c and the container 201d.

When user U checks the calibration curve creation check button (calibration curve information) 312Wd, the control unit 9 refers to the memory unit 8 and controls the sample introduction unit 3b to extract the CBZ standard sample with sequence number 3 from the actual sample holding unit 3a and mix it in container 201d to prepare diluted standard samples of multiple concentrations. The control unit 9 then introduces the diluted standard sample in container 201d with sequence number 10 into the detector 6, causing calibration curve measurement to be performed.

There may be cases where the diluted sample 201c and the empty container 201d are not held in the predetermined positions (sequence numbers 9 and 10) of the sample holding section 3a.
When the control unit 9 detects this state, it displays the holding positions (sequence numbers 9 and 10) of the diluted sample 201c and the container 201d on the holding position information 300. Moreover, the information setting status indicates that sequence numbers 9 and 10 are "diluted sample" and "empty container", respectively.
Therefore, the control unit 9 notifies the user that the samples in each holding position are a diluted sample and a container based on the information set in the information setting status, and prompts the user to place the diluted sample 201c and the empty container 201d.

This notification is not particularly limited, and on the holding position information 300, the holding positions of the diluted sample 201c and the container 201d (sequence numbers 9 and 10) may be displayed as "diluted sample" and "empty container", respectively, and this display may be color-coded or highlighted by flashing or the like.
Also, on the display screen of the display unit 10, a banner or a telop or the like different from the holding position information 300 may be displayed to prompt the user to place a "diluted sample" and an "empty container" at the holding positions (sequence numbers 9 and 10), respectively. Also, a voice may be used to notify the user.

As described above, by selecting a sample on the holding position information 300, the user can easily select whether or not to create a calibration curve, and the calibration curve is automatically created according to the type of sample, eliminating the need for settings for creating the calibration curve and preventing mistakes such as creating an incorrect calibration curve.

In this example, the types of samples in the upper row 300x of the holding position information 300 in FIG. 4 are all determined in advance, preventing the types from being changed erroneously.
That is, as shown in FIG. 6, even if the user U specifies an information setting status for the sample in the upper row 300x (eg, sequence number 3), the control unit 9 invalidates this specification.

In this example, the type of sample (blank, CBZ, etc.) 306 is displayed in the upper row 300x of the holding position information 300 in FIG.
On the other hand, in the lower row 300y, UNK is uniformly displayed as the sample type 306. However, the lower row 300y may display the sample type (e.g., CBZ) designated by the information setting status 312.
As described above, by displaying the sample type 306, the types of samples in the holding positions 302 can be visually grasped all at once on the holding position information 300.

In this example, for samples in any measurement status except for the measurement in progress status 316 in the holding position information 300, it is possible to reset the measurement status to any one of these.
7, for example, for a sample that has already been measured (sequence number 11) or a sample for which the measurement reservation status 314 has been released (sequence number 13), the information setting status 312 or a new measurement reservation status 314 can be specified. For a sample with an unset status 310, the information setting status 312 or the measurement reservation status 314 can be specified as a matter of course.
5, when the user U clicks on the "Clear sample information" button 312Wc, the sample type set in the information setting status 312 is cleared (deleted). In this example, the default setting is to display the unset status 310 with a white circle.

As described above, it is possible to reset the measurement status for any sample in the holding position information 300 that has a measurement status other than the measurement in progress status 316, making it easy to change the settings, for example, to urgently measure a new sample in the position of a sample that has already been measured.

In this example, when the user U selects a specific sample on the holding position information 300, the control unit 9 may display corresponding information about the sample.
For example, if the selected sample is in the information setting status 312 or the measurement reservation status 314, the type of sample can be displayed.
Also, as shown in FIG. 9, if the selected sample has a measured status 318, the measurement results can be displayed.

As described above, by displaying the corresponding information about the selected sample on the holding location information 300, this information can be easily obtained and information about other samples can be prevented from being obtained by mistake.

It goes without saying that the present invention is not limited to the above-described embodiment, but covers various modifications and equivalents within the spirit and scope of the present invention.
The form of the sample holder and the holding position information representing it are not limited, and may be, for example, as shown in FIG. 10, a form in which samples are arranged and held along the circumferential direction of a circular sample holder.
Each measurement status is not limited to being displayed in a different color, and may be highlighted, for example, by blinking.
The sample holders and the holding position information representing them are not limited to being arranged in a single row as in FIG. 3, but may be arranged in a form in which the samples are held along the circumferential direction of a circular sample holder as shown in FIG.

3 Autosampler 3a Sample holder 3b Sample introduction section 6 Detector (measuring device)
7 Data processing device (control device for autosampler)
8 Memory unit 9 Control unit 10 Display unit 100 Liquid chromatograph (automatic measurement system)
201a to 201c Vials (samples)
201d Container for dilution (empty container)
300 Storage location information 302 Storage location 304 Check box (measurement selection information)
306 Sample type 312 Information setting status 312Wd Check button (calibration curve information)
314 Measurement reservation status 316 Measurement in progress status 318 Measurement completed status U User input

Claims (5)

1. A control device for an autosampler including a sample holding unit that holds a plurality of samples in an array and a sample introduction unit that introduces the plurality of samples one by one into a measuring device, the control device having a control unit and a memory unit,
The control unit causes a predetermined display unit to display holding position information indicating holding positions of the plurality of samples in the sample holding unit,
the holding position information includes a sequence number indicating the arrangement order of the samples in the sample holding unit and measurement selection information indicating whether or not a measurement is scheduled;
The control unit of the autosampler control device is characterized in that, when the measurement selection information indicates that a measurement is reserved at the time the current measurement is completed, the control unit controls the sample introduction unit to introduce the samples, for which the measurement selection information indicates that a measurement is reserved, into the measurement device in order of the sequence number from earliest to latest. The control unit of the autosampler control device described in claim 1 transmits to the measurement device measurement conditions corresponding to the type of sample to be next introduced into the measurement device in accordance with the order of the sequence numbers for samples for which the measurement selection information indicates that a measurement reservation has been made. When the user selects the sample on the storage location information,
3. The autosampler control device according to claim 1 , wherein the control unit displays corresponding information regarding the sample . A control device for an autosampler according to any one of claims 1 to 3;
The autosampler;
and the measuring device. 5. The automated measurement system according to claim 4, which is a liquid chromatographic measurement system.

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