JP3532020B2 - Chromatogram check device and chromatogram check method - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a chromatogram check device and a chromatogram check method for determining whether a chromatogram is normal or abnormal.

[0002]

2. Description of the Related Art Conventionally, in a data processing device for chromatography, a printer or the like outputs numerical values such as a chromatogram and a quantitative calculation result based on measurement data received from a detector (see FIG. 6). Therefore, the inspector visually checks this output result to see if the other components do not overlap with the chromatogram, does not mistakenly identify the other component as the target component, and whether the measurement by the detector is normal. The qualitative aspect and the quantitative aspect were checked.

[0003]

However, in the conventional data processing apparatus for chromatography, it is necessary for the inspector to visually check the qualitative surface and the quantitative surface for all the samples. It takes a lot of time to judge whether or not it is normal, which causes deterioration of work efficiency.

An object of the present invention is to provide a chromatogram checking device and a chromatogram checking method capable of efficiently checking chromatograms for a large number of samples.

[0005]

A chromatogram checking device according to a first aspect of the present invention stores check data storing means for storing check data for standard substances and check data for each sample, and the check data storing means. Discrimination means for comparing the check data of standard substances and the check data of each sample to determine whether the chromatogram of each sample is normal or abnormal, and the sample for which the chromatogram is discriminated by this discrimination means And output means for outputting the sample number ,
Check data of reference materials and check of the sample
The check data contains multiple check items.
Therefore, the determination means is different for any check item.
If it is determined to be normal, check other check items.
It is characterized in that it does not judge whether it is normal or abnormal .

Therefore, a large number of chromatograms can be checked by displaying or printing the chromatogram of the sample with the sample number output by the output means and visually checking the presence or absence of abnormalities only for this chromatogram. It can be done efficiently. Well
Acceleration of chromatogram check for each sample
Chromatography for large numbers of samples
It can also speed up the ram check.

Further, in the chromatogram check device according to claim 2, the check data storage means of the chromatogram check device according to claim 1 is further provided with each check item.
The predetermined range relating to the eyes is stored, and the discriminating means stores the mark.
Check data for quasi substances and check data for the sample
It is judged whether the difference in data is within the specified range.
Yes, if it is judged that it is not within the above specified range,
With presence of the abnormality in the chromatogram, wherein the chromatogram of the sample to determine whether it is normal or abnormal.

Further , the chromatogram check according to claim 3
The check device is the chromatogram check according to claim 1 or 2.
Check device, the check data storage means further includes an inspection item.
Stores the specified value for the quantitative calculation result for each eye and
The means further includes the quantitative calculation result of each sample and the predetermined value.
And whether the chromatogram of each sample is normal
It is characterized by determining whether it is abnormal.

Therefore, whether the chromatogram is normal or not
Check the reference data and reference
Sample check data comparison as well as each sample
Comparison of quantitative calculation results with predetermined values for quantitative calculation results
The chromatogram is normal or abnormal.
It is possible to improve the accuracy of the determination as to whether or not

A chromatogram check according to claim 4
The clock device according to any one of claims 1 to 3.
By the output means of the matogram check device, the chroma
Samples related to samples whose togram was determined to be abnormal
Output the number and chromatogram for this sample.
It is characterized by outputting ram.

Therefore, this sample together with the sample number
The chromatogram for
Very fast and easy to determine whether the togram is abnormal
Can be done

Further, the chromatogram check according to claim 5
The locking device is the clock device according to any one of claims 1 to 4.
Check day of the reference material of the matogram check device
Data and the check data of the sample should be at least
Retention time is included, and the determination means
First, the retention time of the standard substance and the
Chromatography of each sample by comparing retention times
Characterized by distinguishing whether the rum is normal or abnormal
And

Here, the chromatogram is judged to be abnormal.
Retention time for standards and samples, if
Most often because the difference between the
Therefore, check the retention time first.
Chroma for multiple samples
Togram check can be performed at high speed.

The chromatogram check according to claim 6
The check method is to check the check data of the standard substance.
First step of reading from the data storage means and each sample
Read the check data from check data storage means
The second step and the first step
Check data of the issued reference material and the second step
Check data of each sample read in
And whether the chromatogram of each sample is normal
The third step of determining whether it is abnormal, and the third step
If the chromatogram was determined to be abnormal in the step,
Sample number for the sample and this sample
A fourth step of outputting a chromatogram, and
Check data of reference materials and check of the sample
The check data contains multiple check items.
In the third step, any check item
If it is determined that the eyes are abnormal, another check
Check whether the item is normal or abnormal.
It is characterized by not breaking.

Therefore, the color of the output sample is
Inspector visually confirms only abnormality in matogram
Checking a large number of chromatograms by checking
Can be performed efficiently.

The chromatogram check according to claim 7
The check method is the chromatogram check method according to claim 6.
In the first step of the method, each check item
Read a predetermined range for the check data storage means
Of the reference material in the third step.
Difference between check data and check data of the sample
Is within the specified range, and
If it is judged that it is not within the specified range, chromatograph
The chroma of each sample
To determine whether the togram is normal or abnormal.
Characterize. Furthermore, the chromatogram check according to claim 8.
The check method is the chromatogram check according to claim 6 or 7.
In the first step of the check method, further inspection items
Check the specified value for each quantitative calculation result
Read from the storage means, and in the second step,
In addition, record the quantitative calculation results of each sample in the check data
It is read from the storage device and updated in the third step.
Compare the quantitative calculation results of each sample with the above specified value
The chromatogram of each sample is normal or abnormal
It is characterized by determining whether or not. Furthermore, claim 9
The method for checking chromatograms described in the above is the method of claim 6-8.
Check the chromatogram check method described in paragraph 1
Check data of the reference material and the sample
At least the retention time must be included in the check data.
Is included in the third step, and
Retention time of quasi-substance and retention of each sample
The chromatogram of each sample is correct
It is characterized by determining whether it is normal or abnormal.

[0017]

1 is a block diagram of a chromatogram check device 10 according to an embodiment of the present invention.
Shows the state of being connected. The chromatogram check device 10 includes four detectors 30a to 30d.
Are connected, and each of the detectors 30a to 30d can measure 50 samples at a time. That is, in the detector 30a, the sample number 00
1-050, sample number 0 in detector 30b
51 to 100, the detector 30c can measure the sample numbers 101 to 150, and the detector 30d can measure the sample numbers 151 to 200.

Each of the detectors 30a to 30d measures each sample and outputs the measured data as a voltage to the chromatogram check device 10.

FIG. 2 is a block diagram of the chromatogram check device 10 according to the embodiment of the present invention. The chromatogram check device 10 includes a processing device 12 that controls the entire device and performs a chromatogram check described later.
An A / D conversion unit 14, a storage unit 16, an input unit 18, a printer 20, and a display unit 22 are connected to each.

Here, the A / D conversion section 14 is connected to the chromatogram check device 10 and includes detectors 30a to 30a.
The measurement data (voltage) output from 30d is converted into digital data.

The storage unit 16 stores a program for controlling the entire chromatogram check device 10, a program for chromatogram check processing, and the like, and stores the measurement data output by the detectors 30a to 30d. The retention time, the peak height, etc. calculated for each inspection item are stored in association with the sample number.

The input unit 18 is a key input device for inputting a predetermined value regarding mass used in the chromatogram check process.

Further, the printer 20 prints a sample chromatogram and numerical values such as quantitative calculation results, and the display unit 22 displays numerical values such as the sample chromatogram and quantitative calculation results. is there.

Next, with reference to FIG. 3, the inspection data receiving process performed in the chromatogram checking device 10 will be described.

First, the measurement data output from the detector 30a is received, that is, the measurement data (voltage) regarding the sample of sample number 001 is received (S10), and is converted into digital data by the A / D conversion unit 14. Here, first, the measurement data output from the detector 30a relates to the sample of sample number 001.

Next, the data used in the chromatogram check process is calculated based on the received measurement data (S11). That is, the retention time (RT), peak height (HIGHT) and peak area of epinephrine (E), norepinephrine (NE), dopamine (DA) were calculated, and (peak area) / (peak height)
To calculate. Then calibrate the standards,
The mass of epinephrine (E), norepinephrine (NE), and dopamine (DA) contained in the sample by identifying the sample based on the result (quantitative calculation result)
To calculate. Since the sample number 001 is assigned to the standard substance, the calculated data (retention time (R
T), peak height (HIGHT), peak area, (peak area) / (peak height), etc. become reference data in the chromatographic check process.

Next, the calculation data calculated based on the measurement data received from the detector 30a is sampled with the sample number 001.
It is stored in the storage unit 16 in association with (S12).

Next, with respect to the detector currently receiving data, that is, the detector 30a, the sample number 001
It is determined whether or not the measurement data has been received for all the samples up to 050 (S13). here,
At this time, since only the measurement data regarding the sample with the sample number 001 is received, the measurement data regarding the sample numbers 002 to 050 are sequentially received. Since the sample number 002 is given to the controlled substance, the calculated data regarding the controlled substance is used for finding an abnormality in the detectors 30a to 30d.

In the processing of S13, the detector 30a
When it is determined that the measurement data has been received for all the samples of sample numbers 001 to 050, the measurement data of the samples of the sample numbers 051 to 100 regarding the detector 30b is received as in the case of the detector 30a. , Sample number 10 for detector 30c
Receive measurement data of 1 to 150 samples, detector 3
For 0d, the measurement data of the samples of sample numbers 151 to 200 are received. Regarding the detector 30b, the sample of sample number 051 is a standard substance, the sample of sample number 052 is a controlled substance, and for the detector 30c, the sample of sample number 101 is a standard substance and the sample of sample number 102 is controlled. Regarding the detector 30d, the sample with the sample number 151 is the standard substance, and the sample with the sample number 152 is the controlled substance. When this process ends, S14
In the process of (3), it is determined that the measurement data has been received for all the detectors, that is, the detectors 30a to 30d, and the measurement data receiving process ends.

Next, the chromatogram checking process performed by the chromatogram checking device 10 will be described with reference to FIG.

First, the chromatogram of the sample (sample numbers 001 to 050) related to the detector 30a is checked. That is, the calculation data (check data) of the standard substance (sample number 001) stored in the storage unit 16 is read (S20), and the calculation data (check data) of the sample of sample number 003 is read. (S21).

Next, the retention time (R) of the standard substance for a predetermined inspection item, for example, epinephrine (E), is measured.
T) and the retention time (RT) difference of the sample of sample number 3 are determined whether they are within a predetermined range (S22), and when it is determined that they are not within the predetermined range, the chromatogram is abnormal. And the sample number of this sample is stored in the storage unit 16 (S2
3). The predetermined range for the difference between the retention time (RT) of the standard substance and the retention time (RT) of the sample is input in advance from the input unit 18, and is stored in the storage unit 16.
Is stored in. In addition, the same applies to the predetermined range regarding the difference between (peak area) / (peak height) of the standard substance and the (peak area) / (peak height) of the sample, and the predetermined value (high value and low value) related to mass described below It is input in advance from the input unit 18 and stored in the storage unit 16.

On the other hand, when it is judged that the difference between the retention time (RT) of the standard substance and the retention time (RT) of the sample is within a predetermined range in the process of S22, (peak area) / (peak area) of the standard substance / It is determined whether the difference between (peak height) and (peak area) / (peak height) of the sample of sample number 003 is within a predetermined range (S24), and it is determined that the difference is not within the predetermined range. In some cases, there is an abnormality in the chromatogram,
The sample number of this sample is stored in the storage unit 16 (S23).

On the other hand, in the above-mentioned processing of S24, (peak area) / (peak height) of the standard substance and (peak area) / (peak height) of the sample of sample No. 003
If it is determined that the difference between the two is within a predetermined range, is the quantitative calculation result of the sample of sample number 003 related to epinephrine (E) equal to or greater than a predetermined value (high value) (S2
5) Whether or not it is less than or equal to a predetermined value (low value) (S26) is determined. It is determined that there is an abnormality in the chromatogram, and the sample number of this sample is stored in the storage unit 16 (S23).

On the other hand, if it is judged in the process of S25 that the value is not less than the predetermined value and in the process of S26 that it is not more than the predetermined value, the chromatogram of the sample of sample number 3 concerning epinephrine (E) is normal. To be judged.

Next, it is judged whether or not the check of the chromatogram has been completed for all the designated inspection items, that is, norepinephrine (NE) and dopamine (DA) (S27). In this case, since the chromatogram check for norepinephrine (NE) and dopamine (DA) has not been completed yet, the chromatogram check is performed by performing the same processing as that for epinephrine (E) (S22-). S26).

When it is judged in the above-mentioned processing of S27 that the check of the chromatograms for all the designated inspection items is completed, the chromatography of all the samples (sample numbers 003 to 050) relating to the detector 30a is performed. It is determined whether the gram check is completed (S28). In this case, sample number 00
Since only the check of the chromatogram for the sample of No. 3 has been completed, the chromatogram of the samples of sample numbers 004 to 050 is also checked by performing the same processing (S22 to S27) as the sample of sample number 003. .

In the processing of S28 described above, the detector 30
All samples related to a (sample numbers 003 to 050)
When it is determined that the check of the chromatogram of No. 1 is completed, the sample number of the sample in which the chromatogram stored in the storage unit 16 is determined to be abnormal and the chromatogram of this sample are printed by the printer 20 (S29). ).

Further, as shown in FIG. 5, the measurement result of each sample is displayed on the display unit 22 in association with the sample number (S30). Here, “displayed as a message on this display” indicates what number of check items in the chromatogram check process was determined to be abnormal, and is displayed corresponding to sample number 007. , The sample of sample number 007 indicates the third check item, that is, it is determined as abnormal in the process of S25, and it is displayed corresponding to the sample number 012. This indicates that the first check item, that is, an abnormality is determined in the process of S22.

Samples related to the detector 30b (sample numbers 053 to 100), samples related to the detector 30c (sample numbers 103 to 150), detector 30d.
The chromatogram is similarly checked for the samples (sample numbers 153-200) related to.

Therefore, the inspector visually inspects the output result only for the sample printed as anomalous, does not overlap other components in the chromatogram, is the other component erroneously identified as the target component, etc. It is sufficient to check the qualitative surface and the quantitative surface, and it is possible to efficiently check the chromatogram for many samples.

Further, by checking the message on the display, it is possible to know in which check item the sample judged to be abnormal is judged to be abnormal.

In the above embodiment, it is judged whether the chromatogram is normal or abnormal, and the sample number of the sample judged to be abnormal and the chromatogram of this sample are printed. However, it is also possible to print or display the sample number of the sample judged to be normal and the chromatogram of this sample. In this case, it is also possible to print or display the chromatograms of the samples judged to be normal by superimposing them.

[0044]

According to the chromatogram check device of the present invention, since the sample number of the sample whose chromatogram is determined to be abnormal by the determining means is output, the chromatogram relating to the sample of the sample number output by the output means. Is displayed or printed, and the inspector visually confirms whether or not there is an abnormality only with respect to this chromatogram, so that a large number of chromatograms can be efficiently checked.

Further, when the predetermined value (high value and low value) for each test item is also used for judging whether the chromatogram is normal or abnormal, the accuracy of the judgment can be further improved.

Further, when the output means outputs the chromatogram for this sample together with the sample number of the sample for which the chromatogram is determined to be abnormal, it is further efficiently judged whether or not the chromatogram is abnormal. be able to.

When it is determined by the discriminating means that any one of the check items is abnormal and the other check items are not determined to be normal or abnormal, the chromatogram of each sample is checked. In addition to being able to speed up, it is possible to speed up checking of chromatograms for a large number of samples.

In the case where the determination means first compares the retention time of the standard substance and the retention time of each sample to determine whether the chromatogram of each sample is normal or abnormal, a large number of samples are used. The check of the chromatogram regarding can be performed at high speed.

Furthermore, according to the chromatogram checking method of the present invention, a large number of chromatograms can be efficiently checked by the inspector visually confirming the presence or absence of abnormalities only with respect to the chromatogram of the output sample. be able to.

[Brief description of drawings]

FIG. 1 is a diagram showing a state in which a detector is connected to a chromatogram check device according to an embodiment of the present invention.

FIG. 2 is a block configuration diagram of a chromatogram check device according to the embodiment of the present invention.

FIG. 3 is a flowchart for explaining a measurement data receiving process in the chromatogram checking device.

FIG. 4 is a flowchart for explaining a chromatogram check process in the chromatogram check device.

FIG. 5 shows a state of displaying a list of measurement results of each sample.

FIG. 6 shows a state in which numerical values such as a chromatogram and quantitative calculation results are printed by a printer.

[Explanation of symbols]

10 ... Chromatogram checking device, 12 ... Processing device,
14 ... A / D conversion section, 16 ... storage section, 18 ... input section, 2
0 ... Printer, 22 ... Display unit, 30a to 30d ... Detector.

Continuation of front page (56) References JP-A-56-90259 (JP, A) JP-A-49-123398 (JP, A) JP-A-61-25058 (JP, A) JP-A-62-263464 (JP , A) JP 5-322869 (JP, A) JP 6-324029 (JP, A) JP 5-264533 (JP, A) JP 5-93690 (JP, A) JP 62-121359 (JP, A) JP-A-3-105248 (JP, A) JP-A 64-86060 (JP, A) (58) Fields investigated (Int.Cl. ⁷ , DB name) G01N 30/86

Claims (9)

(57) [Claims] 1. The check data storage means for storing the check data of the standard substance and the check data of each sample is compared with the check data of the reference substance and the check data of each sample stored in this check data storage means. comprising a determining means for chromatogram of each sample to determine whether it is normal or abnormal, and output means for outputting a sample number related to a sample chromatogram is determined as abnormal by the determining means, said reference material Check data and check of the sample
Check data includes multiple check items.
Therefore, the determination means is different for any check item.
If it is determined to be normal, check other check items.
Chromatogram check device, which does not judge whether it is normal or abnormal . 2. The check data storage means further comprises:
A predetermined range regarding check items is stored, and the determination means is provided.
Is the check data of the standard substance and the sample
Whether the difference in check data is within the above specified range
When a judgment is made and it is judged that it is not within the predetermined range
Has an abnormality in the chromatogram,
The chromatogram of each sample is normal or abnormal
The chromatograph according to claim 1, characterized in that
Gram check device. 3. The check data storage means further stores a predetermined value relating to a quantitative calculation result for each test item, and the discrimination means further compares the quantitative calculation result of each sample with the predetermined value. 2. It is determined whether the chromatogram of is normal or abnormal.
Or the chromatogram check device described in 2 . Wherein said output means, to any of the claims 1-3, characterized by outputting a chromatogram for this sample and outputs the sample number for the sample chromatogram is judged to be abnormal Chromatogram check device described. 5. The check data of the standard substance and the check data of the sample include at least a retention time, and the determination means first compares the retention time of the standard substance and the retention time of each sample. The chromatogram check device according to any one of claims 1 to 4, wherein the chromatogram of each sample is determined to be normal or abnormal. 6. A first step of reading the check data of the standard substance from the check data storage means, a second step of reading the check data of each sample from the check data storage means, and a read step in the first step. A third step of comparing the check data of the standard substance with the check data of each sample read in the second step to determine whether the chromatogram of each sample is normal or abnormal; and a fourth step of outputting a chromatogram for the sample number and the sample about a sample chromatogram is determined as abnormal in the third step, Choi check data and the samples of the reference material
Check data includes multiple check items.
In the third step, any check item
If it is determined that the eyes are abnormal, another check
Check whether the item is normal or abnormal.
Chromatogram check method characterized by not 7. In the first step, each chip is further
Check data is stored in the specified range for check items.
Read from the means, and in the third step,
Check data of reference materials and check of the samples
Judge whether the difference in data is within the specified range.
Yes, if it is judged that it is not within the above specified range,
By assuming that there is an abnormality in the chromatogram, each sample
Whether the chromatogram of the sample is normal or abnormal
7. The chromatogram according to claim 6, wherein
Check method. 8. The further inspection in the first step
Check the specified values for the quantitative calculation results for each item
Data from the data storage means, and the second step
In addition, the quantitative calculation results of each sample are shown in the check date.
Read out from the data storage means, and in the third step
Furthermore, compare the quantitative calculation results of each sample with the specified value.
The chromatogram of each sample is normal or abnormal
It is determined whether or not
How to check the chromatograms listed. 9. The check data of the standard substance and the
The sample check data should include at least the retention
Included in the third step.
First, the retention time of the standard substance and each sample
Of each sample to compare the retention time
To determine whether the togram is normal or abnormal.
9. The chroma according to any one of claims 6-8.
Togram check method.