JP2021063791A - Liquid chromatography apparatus - Google Patents

Abstract

To provide a liquid chromatography apparatus capable of improving the work efficiency while reducing the burden on a user and avoiding unnecessary adjustments by automatically determining whether or not the adjustment of the apparatus is required and adjustments are made automatically when beginning measurement.SOLUTION: The liquid chromatography apparatus has a control unit for measuring the same sample or different sample in the same column under predetermined measurement conditions. The control unit is configured so as to, when the current measurement has finished and before starting the next measurement, compare the predetermined comparison conditions among the measurement conditions of the current measurement with the comparison conditions in the measurement conditions of the next measurement. When the comparison results match within a given threshold, the next measurement is executed without adjusting the apparatus, and when there is found a mismatch exceeding the threshold, an adjustment of the apparatus is executed as determined according to the threshold value.SELECTED DRAWING: Figure 2

Description

The present invention relates to a liquid chromatograph device.

When measuring with a liquid chromatograph (HPLC) device, if the sample changes, the analysis (measurement) conditions need to be changed, and the device needs to be prepared and stabilized in advance (conditioning). The reason is, for example, (i) when the liquid composition to be sent to the column changes, it takes time to replace the liquid in the flow path (replacement), and (ii) when the measurement conditions change, the column changes to the new measurement conditions. It is necessary to send the liquid until it is balanced (equilibrium), and (iii) when the measurement wavelength changes, the wavelength position etc. is moved in the detector, so it is necessary to wait until the state of that position stabilizes (iii). This is because there is a drift factor).
On the other hand, there is a demand for automating the measurement and adjustment of a liquid chromatograph device, and a technique for improving work efficiency by allowing the user to select a predetermined preparation process such as pump purging and omitting or shortening the time has also been developed. (Patent Document 1).

Japanese Patent No. 5481520

However, in the case of the above-mentioned technique, the user must determine a process of omitting or shortening the preparation process, which complicates the work and goes against automation.
On the other hand, if a certain preparatory process is uniformly and automatically performed without making this judgment, for example, a waiting time is required for the preparatory process even though almost no conditioning is required, and the effective time for performing the actual measurement is reduced. , There is a problem that work efficiency is lowered.

Therefore, the present invention has been made to solve the above-mentioned problems, and at the time of measurement, the presence or absence of adjustment of the device is automatically determined, and further adjustment is automatically performed, so that the burden on the user is reduced and the burden on the user is reduced. An object of the present invention is to provide a liquid chromatograph device capable of avoiding unnecessary adjustments and improving work efficiency.

In order to achieve the above object, the liquid chromatograph device is provided with a control unit and measures the same sample or different samples on the same column under predetermined measurement conditions. The control unit has completed the current measurement. When starting the next measurement, a predetermined comparison condition among the measurement conditions of the current measurement is compared with the comparison condition in the measurement condition of the next measurement, and the comparison result is within a predetermined threshold value. In the case of a match, the next measurement is performed without adjusting the device, and when the measurement exceeds the threshold value and the mismatch is made, the adjustment of the device determined according to the threshold value is executed. ..

According to this liquid chromatograph device, the control unit compares the comparison conditions of the current and next measurements, automatically determines whether or not the device is adjusted based on the match or mismatch of the comparison results, and also automatically performs the adjustment. , The burden on the user is reduced, unnecessary adjustments are avoided, and the effective time for performing the actual measurement is increased, so that the work efficiency can be improved.

In the liquid chromatograph apparatus of the present invention, the comparison condition may include one or more selected from the group of liquid feeding conditions or liquid composition, measurement wavelength, and measurement temperature of the column.
According to this liquid chromatograph device, conditions that greatly affect the presence or absence of adjustment of the device are selected, so that comparison can be performed reliably.

In the liquid chromatograph apparatus of the present invention, the adjustment of the apparatus may include one or more selected from the group of first time standby, noise check, and drift check.
According to this liquid chromatograph device, since the item having a large effect is selected as the adjustment of the device, the adjustment can be surely performed.

In the liquid chromatograph apparatus of the present invention, the control unit determines whether or not the adjustment of the apparatus has been performed within the second time, and in the case of a negative determination, a solution corresponding to the measurement of a predetermined sample in the column. May be sent and a standard sample of the sample may be measured to confirm the normality of the apparatus.
According to this liquid chromatograph device, it is possible to prevent the stability of the device from being lowered because the adjustment is not performed within the second time, which is a daily span, for example.

In the liquid chromatograph apparatus of the present invention, when the liquid feeding of the column is stopped, the control unit may wait for a third hour after starting the liquid feeding of the column and then perform the comparison.
According to this liquid chromatograph device, the control unit determines whether or not the liquid feeding of the column is stopped, and if the liquid feeding is stopped, the liquid feeding is started and the liquid feeding is waited for a third time before comparison. , It is possible to suppress the measurement in an unstable state of the column before the lapse of the third hour.

In the liquid chromatograph apparatus of the present invention, when the fourth time elapses from the end of the current measurement to the start of the measurement of the next measurement, the control unit may reduce the liquid feed flow rate of the column. ..
According to this liquid chromatograph device, it is possible to suppress the waste of the mobile phase by reducing the flow rate to the extent that the stability of the column is not impaired.

The liquid chromatograph device of the present invention further includes a storage unit that previously stores a plurality of measurement conditions for each measurement as continuous measurement conditions in the order of measurement, and when the control unit receives a predetermined signal to perform continuous measurement. , The continuous measurement condition may be acquired, and the measurement corresponding to each of the measurement conditions may be continuously and automatically performed with reference to the comparison condition.
According to this liquid chromatograph device, it is possible to automatically perform a plurality of measurements stored in advance in the order of measurement and automatically determine the presence or absence of adjustment in the next measurement following one measurement.

In the liquid chromatograph apparatus of the present invention, the control unit is determined to perform continuous measurement based on the second continuous measurement condition after a lapse of a predetermined time after executing the measurement under the first continuous measurement condition. When the signal is received, when the predetermined time exceeds the predetermined time threshold, the adjustment of the apparatus is promoted regardless of the comparison condition in the last measurement condition of the first continuous measurement condition, and the predetermined time is reached. Does not exceed a predetermined time threshold, and the comparison condition in the last measurement condition of the first continuous measurement condition is compared with the comparison condition in the first measurement condition of the second continuous measurement condition. Then, it may be determined whether or not the device is adjusted.
According to this liquid chromatograph device, after the continuous measurement of the immediately preceding group is completed, if it is desired to continuously measure the next group beyond the time threshold such as the passage of several days, the time has passed and immediately before. Since there is a high possibility that the condition has changed from the continuous measurement conditions of, the device can be forcibly adjusted. Further, when the time does not elapse after the continuous measurement of the immediately preceding group is completed and the time threshold value is not exceeded, the presence or absence of adjustment in the continuous measurement of the next group can be automatically determined.

According to the present invention, a liquid chromatograph device capable of automatically determining the presence or absence of adjustment of the device at the time of new measurement, reducing the burden on the user, avoiding unnecessary adjustment, and improving work efficiency can be obtained. Be done.

In the liquid chromatograph apparatus of the present invention, the control unit determines whether or not the sample is properly set before performing the next measurement after the comparison, and when the sample is set appropriately. The following measurement may be carried out.
According to this liquid chromatograph device, since the measurement is performed when the sample is properly placed, it is possible to prevent the measurement from being performed even though the sample is improperly placed. Further, when the sample is not installed within the time, it is possible to suppress the consumption of the mobile phase due to the lapse of wasted time by ending the measurement.

In the liquid chromatograph apparatus of the present invention, when the time until the sample is properly set exceeds the threshold value, a predetermined stability of the apparatus may be determined.
According to this liquid chromatograph device, it is possible to avoid measuring when the device is unstable due to a long time until it is set, and to measure when the device is stable, so that data reproducibility is improved.

In the liquid chromatograph device of the present invention, when the liquid chromatograph device is activated, the control unit performs comparison of the comparison conditions and execution of the next measurement or adjustment of the device in the next measurement. It may be continuously and automatically executed as an automatic measurement.
According to this liquid chromatograph device, when an input for activating this device (for example, "one-click" such as an enter button on a keyboard) is performed, comparison conditions are compared and the next measurement is executed in the next measurement. Alternatively, the adjustment of the device can be automatically performed, and the user does not need to instruct each time during that time, and the measurement can be automatically performed until the end of the measurement.

In the liquid chromatograph apparatus of the present invention, the control unit performs the automatic measurement before executing the next measurement, compares the comparison conditions, and adjusts the apparatus as necessary. You may judge whether or not the sample is installed.
According to this liquid chromatograph device, in automatic measurement, if the sample is properly installed, it proceeds to the next measurement by judging whether or not the sample is installed, and the next next sample is also automatically measured. Can be measured.

In the liquid chromatograph apparatus of the present invention, the determination as to whether or not the sample is in an installed state may be an instruction by the user or a determination based on a predetermined condition by the control unit.
According to this liquid chromatograph device, the installation state of the sample can be automatically determined by the user's judgment through a person or by the control unit.

It is a figure which shows the structure of the liquid chromatograph apparatus which concerns on embodiment of this invention. It is a figure which shows the data structure of the table including the comparison condition and the adjustment item of an apparatus. It is a figure which shows the automatic adjustment processing flow of the apparatus performed by a control unit. It is a figure which shows the mode which performs a plurality of measurements continuously and automatically based on the continuous measurement condition stored in the storage part. It is a figure which shows the subroutine in the automatic adjustment processing flow of a device performed by a control unit.

Hereinafter, embodiments of the present invention will be described with reference to the drawings.
FIG. 1 is a diagram showing a configuration of a liquid chromatograph device 100 according to an embodiment of the present invention.
The liquid chromatograph device 100 includes a data processing device (control unit) 7 that controls the whole, a mobile phase (mixed solution of eluent and solvent) 1, a pump 2 that sends the mobile phase 1, and an autosampler 3 that injects a sample. A column 4 for separating components, a column oven 5 for keeping the column 4 at a constant temperature, a detector 6 for detecting the separated components, and a display unit 10 are provided.
The data processing device 7 is composed of a computer having a control unit (CPU) 9 for executing analysis and analyzing the analysis result, and a storage unit (hard disk or the like) 8 for storing the analysis result or the analysis result. The display unit (monitor) 10 displays the analysis result and the analysis result.

The detector 6 has an element for detecting the signal strength, and detects the signal strength with respect to time. As the detector, it is also possible to use a three-dimensional detector having a plurality of detection elements and capable of simultaneously acquiring at a plurality of wavelengths.
The sample is injected from the injector (not shown) of the autosampler 3, passes through the column 4 together with the mobile phase 1 sent from the pump 2, and is separated into various components in the sample.
The sample separated into the components is detected by the detector 6. The signal of the detector 6 is sent to the data processing device 7 to perform data processing.
The column 4 is an apparatus generally used as a separation unit for separating the components of the sample existing in the mobile phase 1. The column 4 includes a tessellation column, a monolith column, and the like. As the column packing material for the column 4, various types such as an adsorption type, a distribution type, and an ion exchange type can be used. It is desirable that the column 4 is installed in the column oven 5 so that the column 4 can be kept at a constant temperature and the samples can be separated with good reproducibility.

In order to perform quantitative analysis or qualitative analysis of the sample, the storage unit 8 stores measurement conditions for each type of sample, calibration curve data, and the like.
Further, the storage unit 8 stores a predetermined threshold value for the result of comparing the predetermined comparison conditions among the measurement conditions for the current measurement and the next measurement. Further, when the value exceeds this threshold value and there is a mismatch, the adjustment content of the device determined according to this threshold value is stored.

Specifically, as shown in FIG. 2, in this example, the comparison conditions are the column liquid feeding conditions (flow rate of mobile phase), liquid composition (mixing ratio of eluent and solvent in mobile phase), measurement wavelength, and measurement wavelength. And the measured temperature.
The items for adjusting the device include a predetermined first hour standby, noise check, and drift check. Of these, the first hour standby is a liquid feed stabilization standby, a temperature arrival standby, and a lamp stabilization standby. There is one.

Then, the adjustment item of the apparatus is stored in the table 6T for each combination of whether the comparison result of each item of the comparison condition matches or does not match.
Specifically, for example, as pattern 2 of the comparison result, when the liquid feed conditions of the column do not match (x in FIG. 2) and the measurement wavelength and the measurement temperature match, the liquid feed stabilization is an item for adjusting the device. The table 6T is set to perform standby, noise check, and drift check (◯ in FIG. 2).
Hereinafter, as patterns 3 to 5 of the comparison result, items for adjusting the device when predetermined comparison conditions are different are set.
In pattern 1, all the comparison results match, and the adjustment item of the device is not set, so that adjustment is unnecessary.

On the other hand, the threshold value on which the comparison results of the comparison conditions are considered to match is stored in the storage unit 8 as follows.
The threshold for matching the liquid feeding conditions (flow rate of the mobile phase) and the liquid composition (mixing ratio of the eluent and the solvent in the mobile phase) of the column is when the flow rate and the mixing ratio of the mobile phase are within a predetermined range. The threshold value for matching the measurement wavelength and the measurement temperature is when the measurement wavelength and the measurement temperature are within a predetermined range, respectively. The measured temperature is an actually measured value, and the other comparison conditions are values specified as measurement conditions.
Further, in the first hour standby, the liquid feed stabilization standby waits for a predetermined time after changing the liquid feed conditions. The temperature arrival standby waits for a time until the target temperature set under the following measurement conditions is reached within a predetermined range. The lamp stabilization standby waits for a predetermined time after changing the measurement wavelength.
The liquid feed stabilization standby time may be further changed depending on the device state (whether or not the liquid feed pump is stopped, whether or not the mixing ratio is the same).

Next, with reference to FIG. 3, the automatic adjustment process of the device performed by the control unit 9 will be described.
First, the control unit 9 determines whether or not the stop time of the liquid chromatograph device 100 (hereinafter, appropriately referred to as “device”) exceeds one day (step S2). If Yes in step S2, the control unit 9 appropriately executes full-scale adjustments such as purging and cleaning (step S4). Here, the full-scale adjustment is an adjustment item different from the adjustment of the apparatus in the present invention, and in the present embodiment, it is a more severe adjustment item (purge, cleaning of the pump plunger, etc.).
That is, in the present embodiment, the adjustment of the device is lighter than the full-scale adjustment, but of course, it can be applied to the more severe adjustment.
Further, in the present embodiment, it is premised that the same sample or different samples are measured on the same column under predetermined measurement conditions.

If No in step S2 and if step S4 is completed, the control unit 9 determines whether or not the device has been adjusted within the second time (step S6). The second hour is, for example, one day, and if not adjusted during this period, the stability of the device may decrease. If Yes in step S6, the process proceeds to step S12. If No in step S6, the control unit 9 measures the QC sample (step S8) and determines whether or not the measurement result of the QC sample is normal (step S10).
A QC sample is a type of standard sample, including an internal standard and a standard sample. By measuring the QC sample, it is possible to confirm whether the peak height of the standard sample is equal to or higher than a predetermined value, that is, the normality of the measurement result of the QC sample. Of course, if it is a standard sample, it is not limited to a QC sample.

If Yes in step S10, the device can be regarded as normal, and the process further proceeds to step S12. If No in step S10, the control unit 9 considers that the device is not normal and proceeds to step S30.
In step S12, the control unit 9 determines whether or not the liquid feeding of the column is stopped. If the liquid feeding is stopped, the column may not be in equilibrium and the measurement may become unstable. Then, if Yes (stopped) in step S12, the control unit 9 starts the liquid feeding in step S14, waits for a third time, and then proceeds to the next step S16. This equilibrates and stabilizes the column. The third time is, for example, about 5 minutes.
On the other hand, if No in step S12, the process proceeds to step S16 as it is.

In step S16, when the current measurement is completed and, for example, there is a next measurement instruction by user input or automatic processing, the control unit 9 acquires the measurement conditions (including comparison conditions) for the next measurement.
Next, in step S18, the control unit 9 compares the comparison condition of the current measurement with the comparison condition of the next measurement, and determines whether or not they match within the threshold value. The "comparison condition" and "threshold value" are as described above.
If Yes in step S18, the control unit 9 executes the next measurement without adjusting the device (step S22).
If No in step S18, the control unit 9 adjusts the device (step S20). For example, as shown in Table 6T of FIG. 2, as comparison conditions, when the liquid feeding conditions (flow rate of the mobile phase) and the liquid composition (mixing ratio) of the column do not match, as pattern 2, the liquid feeding stabilization standby and the liquid feeding stabilization standby and Noise check and drift check are automatically performed as adjustment items.

When the control unit 9 makes a judgment in step S16, if the next measurement instruction is an automatic process instead of the user's input, an input for the user to activate the present device before step S2 (for example, an enter button on the keyboard). By performing "one-click" or the like), steps S2 to S20 in FIG. 3 can be automatically performed, and the user does not have to instruct each time during that time, and the measurement can be automatically performed until the end of the measurement (hereinafter,). "Automatic measurement").
When step S20 is completed, the subroutine “sample (sample) installation” is processed as necessary, and then the process proceeds to step S22. The subroutine "sample installation" will be described later with reference to FIG.

When the measurement (next measurement) in step S22 is completed, the control unit 9 determines whether or not there is a next measurement instruction (next to the measurement completed in step S22) (step S24).
If Yes in step S24, the process returns to step S2 unless the measurement is completed in step S30 (No). For example, when "measurement end" is instructed by the user's input, the control unit 9 determines "Yes" in step S30 and ends the measurement.
On the other hand, if No in step S24, the control unit 9 determines whether or not the fourth time has elapsed (step S26), and if Yes in step S26, the flow rate of the column liquid is reduced (step S28). ). On the other hand, if No in step S26, the process returns to step S24.
In the process of this step S26, when the fourth time elapses between the current measurement and the next measurement, the mobile phase is wasted if the liquid feed flow rate under the measurement conditions is continued as it is, so that the column is stable. This is to reduce the flow rate to the extent that the property is not impaired. The fourth hour is, for example, a few minutes.
When step S28 is completed, the process proceeds to step S30.

As described above, the control unit 9 compares the comparison conditions of the current measurement and the next measurement, automatically determines whether or not the device is adjusted based on the matching or disagreement of the comparison results, and automatically performs the adjustment. Since the burden on the user is reduced and the effective time for performing the actual measurement is increased by avoiding unnecessary adjustment, the work efficiency can be improved.
Further, if the control unit 9 determines whether or not the adjustment of the device is performed within the second time, it is possible to prevent the stability of the device from being lowered because the adjustment is not performed within the second time.

Further, if the control unit 9 determines whether or not the liquid feeding of the column is stopped, and if the liquid feeding is stopped, the liquid feeding is started, the liquid feeding is waited for the third hour, and then the comparison is performed, the third hour elapses. It is possible to suppress the measurement when the previous column is unstable.
Further, if the control unit 9 determines whether or not the fourth time has elapsed between the two measurements and reduces the flow rate of the column liquid feed when the fourth time elapses, the flow rate does not impair the stability of the column. It is possible to suppress the waste of the mobile phase by squeezing.

Further, as shown in FIG. 4, the storage unit 8 stores in advance a plurality of measurement conditions for each of the measurements A and B as continuous measurement conditions in the order of measurement, and the control unit 9 sends a predetermined signal to the effect that continuous measurement is performed. Upon reception, continuous measurement conditions may be acquired, and a plurality of measurements A and B corresponding to each of the measurement conditions may be continuously performed with reference to the comparison conditions.
As a result, while automatically performing the measurements of the plurality of measurements A and B stored in advance in the order of measurement, the presence or absence of adjustment in the measurement B next to the measurement A is automatically determined based on the comparison conditions of the measurements A and B. it can. The judgment based on the comparison conditions is as described above.
The "predetermined signal for continuous measurement" is not particularly limited. For example, when the power of the device is turned on and the control unit 9 performs a column liquid feeding operation or a detection lamp lighting operation in the device, the control unit 9 is used. When the pump performs a gradient operation, when the measurement conditions are acquired at the start of measurement, and the like can be mentioned. That is, the instruction is not limited to the user's intention such as turning on the power of the device, and the instruction may be automatically given at a predetermined timing in the device activation process or the like by the control unit 9.

Further, as shown in FIG. 4, the control unit 9 performs continuous measurements C and D based on the second continuous measurement condition after a lapse of a predetermined time after executing the measurements A and B under the first continuous measurement condition. When the predetermined signal of the above is received, when the predetermined time exceeds the predetermined time threshold, the adjustment of the apparatus may be prompted regardless of the comparison condition in the last measurement condition (measurement B) of the first continuous measurement condition. Good.
On the other hand, when the predetermined time does not exceed the time threshold value, the control unit 9 sets the comparison condition in the last measurement condition of the first continuous measurement condition and the first measurement condition (measurement C) in the second continuous measurement condition. The presence or absence of adjustment of the device may be determined by comparing with the comparison conditions.

In this way, after the continuous measurement A and B of the immediately preceding group are completed, if it is desired to perform the continuous measurement C and D of the next group beyond the time threshold such as the passage of several days, the time has passed too much. Since there is a high possibility that the condition of measurement B of continuous measurement has changed, the device can be forcibly adjusted. Further, when the time does not elapse after the continuous measurements A and B are completed (for example, during the same day) and the time threshold value is not exceeded, the presence or absence of adjustment in the next continuous measurements C and D can be automatically determined. The judgment based on the comparison conditions is as described above.

Next, the subroutine "sample installation" will be described with reference to FIG.
First, the control unit 9 determines whether or not the sample is installed (set) at a designated position (step S102). If Yes in step S102, the subroutine is terminated and the process proceeds to step S22. On the other hand, if No in step S102, the control unit 9 displays a warning in step S104, waits for installation, and proceeds to step S106.
In step S106, the control unit 9 again determines whether or not the sample is installed at the designated position, and if Yes, the process proceeds to step S110, and if No, the process proceeds to step S108.

The determination in steps S102 and S106 may be an instruction by the user (input by a keyboard or the like) or a determination based on a predetermined condition by the control unit 9.
As a judgment based on a predetermined condition by the control unit 9, signal analysis by a sensor at a sample rack or a vial position can be exemplified.

In step S108, the control unit 9 determines whether or not the time count accumulated from the start time of step S104 is within a predetermined waiting time (for example, 10 minutes). If Yes, the process returns to Step S106, and if No, the process returns to Step S106. It is determined that the measurement is stopped, and the process proceeds to step S28.
In step S110, the control unit 9 determines whether or not the time from the start time of step S104 to the integrated installation is equal to or less than the threshold value, and if Yes, the subroutine is terminated and the process proceeds to step S22. On the other hand, if No, the process proceeds to step S112.
The "threshold value" can be set as the time until the measurement accuracy is lowered when it takes time to set the sample.

In step S112, the control unit 9 confirms the noise and drift, determines whether or not the noise and drift values are equal to or less than a predetermined threshold value, and if Yes, ends the subroutine and proceeds to step S22. On the other hand, if No, it is determined that the measurement is stopped, and the process proceeds to step S28.
Noise can be obtained as, for example, the difference (absolute value) between the maximum value and the minimum value when a signal value (baseline) excluding the sample acquired from the detector 6 is acquired for a predetermined time (1 minute). , This difference is compared with a predetermined threshold. Noise affects the detection sensitivity as the S / N ratio (sample / noise ratio) of the signal value.
The drift is, for example, the slope of the baseline when a signal value (baseline) excluding the sample acquired from the detector 6 is acquired for a predetermined time (1 minute). This slope is obtained by the least squares method by sampling signal values at predetermined time intervals, for example. If the drift is large, it affects the calculated peak height and area value detected by the liquid chromatograph.

In this way, if the subroutine "sample installation" is performed, the measurement is automatically performed in step S22 and subsequent steps when the sample installation is properly performed, so that the measurement is performed even if the sample installation is inappropriate. Can be prevented.
Further, if the sample is not installed within the time according to the determination of S108, it is possible to suppress the consumption of the mobile phase due to the lapse of wasted time by ending the measurement.
Further, when it takes time to install the sample by the processing of S110 and S112, the data reproducibility is improved by checking the state of noise and drift (stability of the device) before measuring.
It should be noted that the specified number of samples are installed at the specified positions, and the waiting time and the threshold count can be determined by various sensors and image analysis.

Further, if it is known in advance that the sample cannot be installed within the waiting time of S106 after the above-mentioned automatic measurement, the subroutine processing can be interrupted manually or automatically. Since the above-mentioned automatic measurement is performed when the analysis is started again, the measurement can be performed under appropriate analysis conditions while shortening the analysis time.

Further, in the above-mentioned automatic measurement, the sample is properly installed by determining whether or not the sample is installed by the above-mentioned subroutine "sample installation" after the end of S18 and S20 and before the start of the measurement of S22. If so, the process proceeds to the next measurement, and the next next sample can be automatically measured in S24.

It goes without saying that the present invention is not limited to the above embodiments and extends to various modifications and equivalents included in the ideas and scope of the present invention.
For example, the comparison conditions and the adjustment items of the device are not limited to the above.

4 Column 9 Control Unit 100 Liquid Chromatographer

Claims (13)

A liquid chromatograph device that has a control unit and measures the same sample or different samples on the same column under predetermined measurement conditions.
When the current measurement is completed and the next measurement is started, the control unit sets a predetermined comparison condition among the measurement conditions of the current measurement to the comparison condition in the measurement condition of the next measurement. Compare with
If the comparison results match within a predetermined threshold, the next measurement is performed without adjusting the device, and if the comparison results exceed the threshold and do not match, the adjustment of the device determined according to the threshold is performed. A liquid chromatograph device characterized by performing. The liquid chromatograph apparatus according to claim 1, wherein the comparison condition includes one or more selected from the group of liquid feeding conditions or liquid composition, measurement wavelength, and measurement temperature of the column. The liquid chromatograph device according to claim 2, wherein the adjustment of the device includes one or more selected from the group of first time standby, noise check, and drift check. The control unit determines whether or not the device has been adjusted within the second time, and determines whether or not the device has been adjusted.
In the case of a negative determination, according to any one of claims 1 to 3, a solution corresponding to the measurement of a predetermined sample is sent to the column, and a standard sample of the sample is measured to confirm the normality of the apparatus. The liquid chromatograph device according to the description. The method according to any one of claims 1 to 4, wherein when the liquid feeding of the column is stopped, the control unit waits for a third time after starting the liquid feeding of the column and then performs the comparison. Liquid chromatograph device. The present invention according to any one of claims 1 to 5, wherein when the fourth time elapses from the end of the current measurement to the start of the measurement of the next measurement, the control unit reduces the liquid feed flow rate of the column. Liquid chromatograph device. Further, a storage unit for storing a plurality of measurement conditions for each measurement as continuous measurement conditions in the order of measurement is further provided.
When the control unit receives a predetermined signal to perform continuous measurement, the control unit acquires the continuous measurement conditions, and continuously and automatically performs the measurement corresponding to each of the measurement conditions with reference to the comparison conditions. The liquid chromatograph device according to any one of claims 1 to 6. When the control unit receives a predetermined signal to perform continuous measurement based on the second continuous measurement condition after a lapse of a predetermined time after executing the measurement under the first continuous measurement condition, the control unit receives a predetermined signal.
When the predetermined time exceeds the predetermined time threshold value, the adjustment of the apparatus is promoted regardless of the comparison condition in the last measurement condition of the first continuous measurement condition.
When the predetermined time does not exceed the predetermined time threshold value, the comparison condition in the last measurement condition of the first continuous measurement condition and the comparison condition in the first measurement condition of the second continuous measurement condition. The liquid chromatograph device according to claim 7, wherein the liquid chromatograph device according to claim 7 is used to determine whether or not the device is adjusted. A claim that the control unit determines whether or not the sample is properly set before executing the next measurement after the comparison, and executes the next measurement when the sample is properly set. The liquid chromatograph device according to any one of 1 to 8. The liquid chromatograph device according to claim 9, wherein when the time until the sample is properly set exceeds a threshold value, a predetermined stability of the device is determined. When the liquid chromatograph device is activated, the control unit automatically continuously and automatically performs the comparison of the comparison conditions, the execution of the next measurement, or the adjustment of the device in the next measurement as automatic measurements. The liquid chromatograph apparatus according to any one of claims 1 to 10, wherein the liquid chromatograph apparatus is performed. In the automatic measurement, the control unit determines whether or not the sample is installed before executing the next measurement, after comparing the comparison conditions and adjusting the device as necessary. The liquid chromatograph apparatus according to claim 11. The liquid chromatograph device according to claim 12, wherein the determination as to whether or not the installation state of the sample is possible is based on an instruction by the user or a determination based on a predetermined condition by the control unit.

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