JP3511471B2 - Liquid chromatograph - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a liquid chromatograph device, and more particularly to a liquid chromatograph device suitable for managing the remaining amount of eluent.

[0002]

2. Description of the Related Art In a chromatographic apparatus, a sample moves together with a mobile phase and passes through a chromatographic unit such as a column to finally separate the components. A liquid chromatograph uses an eluent as its mobile phase. That is, in the liquid chromatograph device,
During the analysis, the eluent is always consumed according to the analysis program.

[0003]

However, in the conventional liquid chromatograph, the consumption amount and the remaining amount of the eluent are not generally taken into consideration when setting the analysis conditions and the analysis program. Therefore, especially in an analysis performed for a long time, a shortage of an eluent may occur during the analysis. In that case, there is a problem that the analysis result that should be originally obtained cannot be obtained and the quality of the analysis result is deteriorated.

An object of the present invention is to provide a liquid chromatograph device capable of ascertaining the analysis quality by grasping the consumption amount and the remaining amount of the eluent.

[0005]

(1) In order to achieve the above-mentioned object, the present invention sends the injected sample to a column together with an eluent by a pump, and detects each component separated by the column as a detector. Detected by, and display the detected peaks of each component as a chromatogram,
In a liquid chromatograph device having data processing means for controlling the pump and column, the data processing means, when performing analysis based on a set analysis program, total consumption of the eluent obtained from the analysis program. The residual amount of the eluent is calculated from the above, and when this residual amount is smaller than a predetermined value, an analysis impossible output is made. With this configuration, it is possible to ascertain the consumption quality and the remaining amount of the eluent, avoid the analysis while the eluent is insufficient, and guarantee the analysis quality.

(2) In order to achieve the above object, in the present invention, the injected sample is sent to a column together with an eluent by a pump, and each component separated by the column is detected by a detector and detected. While displaying the peak of each component as a chromatogram, in the liquid chromatograph apparatus having a data processing means for controlling the pump and column, the data processing means, when performing analysis based on the set analysis program, The number of analyzable times is calculated from the total consumption of the eluent and the remaining amount of the eluent obtained from the above analysis program, and the number of analyzable times is output. With this configuration, it is possible to ascertain the quality of analysis by grasping the consumption amount of the eluent and the number of times the analysis can be performed, avoiding analysis while the eluent is insufficient.

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION The configuration and operation of a liquid chromatograph device according to an embodiment of the present invention will be described below with reference to FIGS. First, the overall configuration of the liquid chromatograph device according to the present embodiment will be described with reference to FIG.

The first to third eluents 10, 12 and 14 are
Each is sucked by the pump 20 and sent to the column 40 via the autosampler 30. Pump 20
Are controlled by the data processing device 70, and the flow rate of the eluent, the switching of the first to third eluents 10, 12, 14 and the mixing of the first to third eluents 10, 12, 14 are performed. And so on. The sample injected by the autosampler 30 is the pump 2
0 to the column 40 together with the eluent.

The sample is separated into each component by a column 40 which is kept at a constant temperature by an oven. Each of the separated components is detected by the detector 50 and is discarded in the waste liquid container 60. The measured value of each component detected by the detector is taken into the data processing device 70, the height and area of the chromatographic peak are calculated, and the result is output to the output device 80 such as a display. An input device 90 such as a keyboard and a mouse is connected to the data processing device 70, and is used for inputting analysis condition setting and analysis program setting. In addition, the data processing device 70 controls the autosampler 30 to control the injection amount of the sample and the temperature of the column 40.

Next, the contents of processing using the data processing device of the liquid chromatograph device according to the present embodiment will be described with reference to FIG. In step 100, the analyst uses the data processing device 70 to set analysis conditions including operating conditions of a chromatographic unit including the pump 20, the autosampler 30, and the column 40. The operating conditions of the chromatographic unit are, for example, the upper and lower pressure limits of the pump 20, the flow rates and mixing ratios of the eluents 10, 12, and 14, the delivery time, the sample suction amount by the autosampler 30, the set temperature of the oven of the column 40, For example, upper and lower temperature limits.

An example of setting analysis conditions according to this embodiment will be described with reference to FIG. The illustrated example is shown in FIG.
The display screen of the display which is an example of the output device 80 shown in FIG. As shown in the figure, “pressure lower limit” and “pressure upper limit” on the display screen are pressure upper and lower limits of the pump 20, and arbitrary numbers can be input by the input device 90. In addition, "time", "mixing ratio", "flow rate"
The mixing conditions of the eluent are shown. In the illustrated example, the eluent 1 is made to flow “100”% during the time “0.0” minutes to “1.0” minutes, and the flow rate at that time is set to “ 0.5 "m
1 / min. In addition, the time “1.
Similarly, eluent 1 is also applied between 0 minute and 2.0 minute.
Flow "100"% and the flow rate at that time is "0.5" ml
/ Min. Furthermore, the time “2.
In the same manner, the eluent 2 is also applied between 0 ”and“ 3.0 ”.
Flow "100"% and the flow rate at that time is "1.0" ml
/ Min. The same applies to the following.

Next, in step 105, the data processing device 70 calculates the consumption amount of the eluent when the analysis conditions set in step 100 are stored in the storage means inside the data processing device 70. That is, the consumption amount of the eluent is calculated by the product of the flow rate of the eluent, the mixing ratio, and the delivery time. For example, in the case of the eluent 1 shown in FIG.
Since the flow rate is 0.5 ml / min and the mixing ratio is 100%, and it is sent from 0 to 2 minutes, the consumption amount is 0.5 x (100
÷ 100) × (2-0) = 1 ml. The calculated consumption amount of the eluent is stored in the storage means inside the data processing device 70.

Here, the data processing device 7 will be described with reference to FIG.
The contents of the analysis conditions stored in the storage means inside 0 will be described. Under the directory of the data processor,
A subdirectory for each analysis condition such as “analysis condition 1” and “analysis condition 2” is provided. The analysis condition set in step 100 is stored in the "operating condition".
Further, the consumption amount of the eluent calculated in step 105 is stored in the “consumption amount of the eluent”. The "other conditions" store the conditions for quantifying chromatographic peaks. For example, whether quantifying chromatographic peaks by peak height or peak area is stored. To be done. The “chromatographic data” stores the chromatographic data of each component detected by the detector 50. In the "data processing result", the quantified result of the chromatographic data stored in the "chromatographic data" by the quantifying method stored in the "other conditions" is stored.

Next, in step 110, the analyst uses the data processing device 70 to set an analysis program including analysis conditions. The analysis program defines the injection amount of the sample, the analysis conditions, etc. for each sample to be analyzed.

Here, a setting example of the analysis program according to this embodiment will be described with reference to FIG. The illustrated example shows a display screen of a display which is an example of the output device 80 shown in FIG. 1. As shown in the figure, the analysis program display screen shows the sample number, sample injection volume (μl), sample injection frequency, sample type, and analysis conditions. Is displayed and you can set each of these items. Regarding the analysis conditions, the analysis conditions used for the analysis are selected from the analysis conditions stored under the directory of the data processing device. In the analysis propriety, the propriety of the analysis is displayed based on the total consumption of the eluent and the calculation result of the number of analyzable times, which will be described later. The "injection volume (μl)" of the sample, "injection frequency", and "analysis conditions" are
It can be set arbitrarily.

Next, in step 115, the analyst designates the sample to be analyzed on the analysis program shown in FIG. The designation method is arbitrary, for example,
All of the samples 1 to 6 may be designated, or it is possible to selectively designate the samples 1, 2, 3, and 5. Here, it is assumed that all of Samples 1 to 6 are selected.

Next, in step 120, the data processing device 70 performs an analysis / determination process. In the analysis determination process, first, in step 121, the data processing device 70 calculates the total consumption amount of the eluent. The calculation of the total consumption of the eluent is performed by searching the directory of the data processing device for the analysis condition of the sample designated in step 110, and then, the consumption of the eluent obtained in step 105 which is stored together with the analysis condition. Read. Then, the sum of the products of the consumption amount of the eluent and the number of injections is obtained.

Next, at step 122, the data processor 70 calculates the number of analyzable times after the calculation of the total consumption of the eluent is completed. That is, the quotient of the remaining amount of the eluent and the total consumption of the eluent calculated in step 121 is obtained. If the calculation result is a decimal number, the number after the decimal point is truncated.
When the calculated number of analyzable times differs for each eluent, the number of analyzable times for each eluent is compared, and the smallest value among them is set as the final number of analyzable times. For example, if the remaining amount of the eluent 1 is 20 ml and the total consumption is 6 ml, then 20/6
Since it is 3.33, the number after the decimal point is rounded down and the number becomes “3” times. As a result of the same calculation, the eluent 2 was "1" times,
When the eluent 3 is “0” times, the smallest value of “0” times of the eluent 3 is the final number of times analysis is possible.

Further, the remaining amount of the eluent after the analysis is performed is calculated. That is, the difference between the remaining amount of the eluent and the total consumption of the eluent is obtained. The remaining amount of eluent is measured using a sensor.
It is automatically measured and loaded into the data processor. The remaining amount information is taken in periodically or upon request from the data processing device. Further, when the eluent is replaced with a new eluent, the input device 90 is used to input the volume of the new eluent, so that the value of the remaining amount of the eluent in the initial state is taken into the data processing device 70. Further, when the eluent is added, the volume of the eluent after the addition is taken into the data processing device 70 from the input device 90. next,
In step 123, the data processing device 70 outputs the calculation result of the number of analyzable times to the output device 80.

Here, an output example of the calculation result of the number of analyzable times according to this embodiment will be described with reference to FIG. The illustrated example shows a display screen of a display which is an example of the output device 80 shown in FIG. 1. As shown in the figure, the “displayable number of times”, “consumption amount” and “remaining amount” for each eluent are displayed on the result display screen. "Number of possible analyzes"
Displays the number of analyzable times determined in step 122. In the "consumption amount", the total consumption amount of each eluent obtained in step 121 is displayed, and the "remaining amount" is displayed.
Indicates the remaining amount of each eluent obtained in step 122.

Next, in step 130, the data processing device 70 determines whether analysis is possible. That is,
It is determined whether or not the number of analyzable times calculated in step 122 is "0" or less. If it is "0" or less, the process proceeds to step 135, and if it is "1" or more, the process proceeds to step 155.

When the number of analyzable times is "0" or less, in step 135, the data processing device 70 displays a message on the display screen as to whether "replenish the eluent". When the replenishment of the eluent is selected, in step 140, the analyst sees the screen of FIG. 6 to confirm which eluent is insufficient and replenishes the eluent more than the insufficient amount. In the case of FIG. 6, since 4 ml of the eluent 3 is insufficient, 4 ml or more of the eluent 3 is replenished. After replenishing the eluent,
Return to step 120 and repeat the calculation.

When the eluent is not replenished,
In step 150, the data processing device 70 displays a message as to whether or not “specify the sample again” on the display screen. If you want to specify the sample again,
Since the number of samples is too large, the process proceeds to step 115 and the sample for which the analysis is to be performed is designated again. If the sample is not designated again, the amount of eluent consumed is large under the set analysis conditions, and the process returns to step 100 and the analysis conditions are set again.

If the result of the determination in step 130 is that analysis is possible, in step 155 the data processing device 7
0 controls the pump 20, the autosampler 30, and the column 40 according to the set analysis conditions and analysis program, and executes the analysis. After the analysis is completed, the chromatographic data analyzed according to the operating conditions is used as the data processing device 70.
And data processing is executed. After the data processing is completed, the chromatographic data, the data processing result and the like are stored in the data processing device 70. Further, after the analysis is completed, in step 160, the data processing device 70 displays a message on the display screen as to whether or not another sample is to be analyzed, and if it is to be executed, the process returns to step 100 to set the analysis condition. Start over. When all the analysis is completed, the work is completed.

Even if the determination in step 130 is “analyzable”, the process can proceed to step 150 to respecify the sample. That is, when the number of analyzable times is, for example, “3 times”, as shown in FIG.
In addition to the analysis of 6 samples of 6, 12 new samples of samples 7-18 can be added to the analysis program. In addition, by changing the “injection frequency” shown in FIG. 5 from “1 time” to “3 times”, the same sample was injected 3 times, repeated measurement was performed, and the results were averaged. It is also possible to perform more accurate measurement. It should be noted that “setting analysis conditions” in step 100 and step 105
The "calculation of the amount of the eluent consumed" in step 1 does not need to be performed each time the analysis is performed, but by performing the process once, the "operating condition" and the "consumption of the eluent" shown in FIG. Since it is stored in “quantity”, this data can be read and used.

As described above, according to the present embodiment, it is possible to accurately grasp the consumption amount of the eluent and the number of times the analysis can be performed, and it is possible to perform the analysis before the eluent is insufficient. It can be prevented and thus the quality of the analysis can be guaranteed.

Next, the configuration and operation of a liquid chromatograph device according to another embodiment of the present invention will be described with reference to FIGS. 7 and 8. The overall configuration of the liquid chromatograph device according to this embodiment is the same as that shown in FIG. Further, the contents of processing using the data processing device of the liquid chromatograph apparatus according to the present embodiment are the same as those in the flowchart shown in FIG. It has been changed.

Here, the processing contents using the data processing device of the liquid chromatograph device according to the present embodiment will be described with reference to FIG. When the "specify sample to be analyzed" process of step 115 shown in FIG. 2 is completed, the process proceeds to "analysis determination" process of step 120A shown in FIG. In step 124 of step 120A, the data processing device 70 subtracts the consumption amount of the eluent obtained in step 105 from the previous remaining amount of the eluent to obtain the remaining amount.

Next, at step 125, the data processor 70 determines whether or not the remaining amount of the eluent is greater than zero. If it is greater than 0, proceed to step 126,
If 0 or less, the process proceeds to step 127. Step 12
In the judgment of 5, if it is larger than 0, step 12
6, the data processing device 70 causes the output device 80 to
"Display output of analysis" OK "" is performed.

The display output in step 126 of this embodiment will be described below with reference to FIG. The illustrated example shows a display screen of a display which is an example of the output device 80 shown in FIG. 1. As shown in the figure, on the display screen of the analysis program, similar to the one shown in FIG. 5, the “number” of the sample, the “injection amount (μl)” of the sample, the “number of injections” of the sample, the sample “Type” and “Analysis condition” are displayed, and “◯” or “X” is displayed in the “Analyzing / Unavailable” column. Here, “◯” is displayed in the “Analyzing / Analyzing” column is the “analytical“ OK ”display output” in step 126.

Further, in the determination at step 125, 0
In the following cases, in step 127, the data processing device 70 performs “analysis“ no ”display output” to the output device 80. In FIG. 8, "x" is displayed in the "Analyzing / Unavailable" column.
Is displayed when “Analysis“ No ”in step 127 is displayed.
Display output ”.

Next, in step 128, the data processing device 70 determines whether or not the calculation has been completed for all the samples, and if not completed, step 12
Return to step 4, repeat the process, and when finished, step 12
The process of 0A is completed, and the process proceeds to the “analyzing possible?” Determination process of step 130 shown in FIG.

FIG. 8 shows a state in which the calculation has been completed for all the samples, and it is possible to analyze samples 1 to 4, but for samples 5 and 6, the remaining amount of the eluent is shown. Is 0 or less, indicating that analysis is impossible. If the analysis cannot be performed, the process proceeds from the determination process of step 130 of FIG. 2 to step 135, and the eluent is replenished in step 140, the sample is reset in step 150, or the analysis condition is reset. become.

In the process in step 125,
Although it is determined whether the remaining amount of the eluent is greater than 0, a threshold value, that is, a lower limit value of the remaining amount of the eluent may be set for the remaining amount of the eluent. . When the remaining amount of the eluent after performing the analysis reaches the threshold value, it is determined that the analysis cannot be performed. The calculation result of the remaining amount of the eluent includes an error, etc.
Even if the remaining amount is more than 0, the remaining amount is actually 0 or less, or due to the mechanism of sucking the eluent,
In some cases, the eluent remaining at the bottom of the eluent bottle may not be completely sucked, so by setting a threshold value,
Further, the reliability can be improved. Further, the threshold value may be set with respect to the consumption amount of the eluent, the total consumption amount of the eluent, and the number of analyzable times.

As described above, according to this embodiment, the consumption amount and the remaining amount of the eluent can be accurately grasped, and the analysis is prevented from being executed in the state where the eluent is insufficient. The quality of the analysis can therefore be guaranteed.

The process shown in step 120 of FIG. 2 or step 120A of FIG. 7 is performed by a set of analysis sample groups (samples of FIG. 5) designated by “designation of analysis sample” of step 115 of FIG. Although the analysis is performed before the analysis of 1 to 6) is started, it is also possible to determine whether or not the analysis can be performed before the analysis of each sample.

In any case, the analysis is not started when all the steps of the analysis program cannot be executed, that is, when the number of possible analyzes is 0 or the remaining amount is 0. In that case, error processing such as outputting a message is executed as to the reason why the analysis cannot be started.

Regarding the error processing, a message indicating the reason why the corresponding step cannot be executed may be output and the analysis may be stopped. Also, output a message indicating the reason why the corresponding step cannot be executed,
You may proceed to the step next to this step. Alternatively,
A message indicating the reason why the corresponding step cannot be executed may be output to prompt the analyst to replenish the eluent. Alternatively, by combining these, the analyst may select whether to stop the analysis, proceed to the next step, or supplement the eluent and continue the analysis.

[0039]

According to the present invention, in a liquid chromatograph, it is possible to ascertain the quality of analysis by grasping the consumption amount and the remaining amount of the eluent.

[Brief description of drawings]

FIG. 1 illustrates an overall configuration of a liquid chromatograph device according to an embodiment of the present invention.

FIG. 2 is a flowchart showing processing contents using the data processing device of the liquid chromatograph device according to one embodiment of the present invention.

FIG. 3 is an explanatory diagram of a setting example of analysis conditions in the liquid chromatograph device according to the embodiment of the present invention.

FIG. 4 is an explanatory diagram of analysis conditions stored inside a data processing device in a liquid chromatograph device according to an embodiment of the present invention.

FIG. 5 is an explanatory diagram of a setting example of analysis conditions in the liquid chromatograph device according to the embodiment of the present invention.

FIG. 6 is an explanatory diagram of an output example of a calculation result of the number of analyzable times in the liquid chromatograph device according to the embodiment of the present invention.

FIG. 7 is a flowchart showing a main part of processing contents using a data processing device of a liquid chromatograph device according to another embodiment of the present invention.

FIG. 8 is an explanatory diagram of a display example of whether or not analysis is possible in a liquid chromatograph device according to another embodiment of the present invention.

[Explanation of symbols]

10, 12, 14 ... Eluent 20 ... Pump 30 ... Autosampler 40 ... Column 50 ... Detector 60 ... Waste liquid container 70 ... Data processing device 80 ... Output device 90 ... Input device

Continuation of the front page (56) Reference JP-A 63-165720 (JP, A) JP-A 1-167659 (JP, A) JP-A 10-82775 (JP, A) JP-A 10-185895 (JP , A) JP 60-168052 (JP, A) JP 4-50770 (JP, A) JP 10-10134 (JP, A) JP 10-123151 (JP, A) JP 2000 -74718 (JP, A) Japanese Patent Publication 1-47744 (JP, B2) (58) Fields surveyed (Int.Cl. ⁷ , DB name) G01N 30 / 00-30 / 96

Claims (2)

(57) [Claims] 1. An injected sample is sent to a column together with an eluent by a pump, each component separated by the column is detected by a detector, and peaks of each detected component are displayed as a chromatogram. In a liquid chromatograph device having data processing means for controlling the pump or column, the data processing means, when performing an analysis based on a set analysis program, the total consumption of the eluent obtained from the analysis program. A liquid chromatograph device, characterized in that the remaining amount of the eluent is obtained from the output, and when the remaining amount is smaller than a predetermined value, analysis is impossible. 2. The injected sample is sent to a column together with an eluent by a pump, each component separated by the column is detected by a detector, and the detected peaks of each component are displayed as a chromatogram. In a liquid chromatograph device having data processing means for controlling the pump or column, the data processing means, when performing an analysis based on a set analysis program, the total consumption of the eluent obtained from the analysis program. A liquid chromatograph device characterized in that the number of analyzable times is calculated from the remaining amount of the eluent and the number of analyzable times is output.