WO2017002156A1 - Dispositif de traitement de sortie de résultat d'analyse et programme de traitement de sortie de résultat d'analyse - Google Patents

Dispositif de traitement de sortie de résultat d'analyse et programme de traitement de sortie de résultat d'analyse Download PDF

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Publication number
WO2017002156A1
WO2017002156A1 PCT/JP2015/068643 JP2015068643W WO2017002156A1 WO 2017002156 A1 WO2017002156 A1 WO 2017002156A1 JP 2015068643 W JP2015068643 W JP 2015068643W WO 2017002156 A1 WO2017002156 A1 WO 2017002156A1
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Prior art keywords
display
analysis result
result output
output processing
cell
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PCT/JP2015/068643
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English (en)
Japanese (ja)
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桐子 松尾
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株式会社島津製作所
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Priority to PCT/JP2015/068643 priority Critical patent/WO2017002156A1/fr
Priority to JP2017525694A priority patent/JP6447727B2/ja
Publication of WO2017002156A1 publication Critical patent/WO2017002156A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/72—Mass spectrometers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/86—Signal analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor

Definitions

  • the present invention is for displaying or printing out analysis results obtained by various analyzers such as a liquid chromatograph, a gas chromatograph, a liquid chromatograph mass spectrometer, and a gas chromatograph mass spectrometer on a display screen. More specifically, the analysis result output processing device and the analysis result output processing program are suitable for displaying or printing out graphs of multi-component quantitative results and chromatograms for a large number of specimens at once.
  • the present invention relates to a result output processing device and an analysis result output processing program.
  • the compound (component) to be measured is determined. Therefore, in mass spectrometers in LC-MS and GC-MS, SIM (selected ion monitoring) measurement or MRM (multiple reaction ion monitoring) measurement targeting mass-to-charge ratios corresponding to many known compounds to be measured can be performed.
  • SIM selected ion monitoring
  • MRM multiple reaction ion monitoring
  • the measurement target compound is repeatedly carried out in the vicinity of the retention time when it elutes from the column. Therefore, chromatogram data for a large number of measurement target compounds is obtained for each sample (specimen), and a peak area value, a quantitative value (concentration), and the like are calculated based on the data.
  • the information of different samples is arranged in the row direction (horizontal direction) and the information of different compounds is arranged in the column direction (vertical direction).
  • a table in which numerical information such as the obtained peak area value and quantitative value is arranged is created, and the table is displayed on the monitor display screen. By displaying such a table, the analyst can check a list of numerical information such as quantitative values for the combination of the sample and the measurement target compound.
  • a graph drawing table is created by arranging the chromatogram (mass chromatogram, extracted ion chromatogram) obtained for each measurement target compound for each sample according to the same matrix arrangement as the numerical information table.
  • a drawing table and a numerical information table are displayed side by side. Thereby, it becomes easy to confirm numerical information such as a quantitative value of a certain measurement target compound in a certain sample and an actually measured chromatogram corresponding to the numerical information.
  • the analyst can easily determine whether each analysis result meets the criteria (within the regulation range) or does not meet the criteria. be able to.
  • the analyst determines what color the analysis result is displayed, so attention will be directed to information that does not need to be focused on, The effect of improving work efficiency is small.
  • a chromatogram for a compound whose quantitative value exceeds the reference value is surrounded by a rectangular frame of a specific color so that it can be easily distinguished from others.
  • the reference value is not limited. I don't know if it exists. If there is only one reference value for determining the quantitative value, there is not much trouble, but if the reference value is set in multiple stages, it is inconvenient if you do not immediately know which reference value is exceeded. Often.
  • the present invention has been made in view of the above problems, and its main purpose is numerical information that an analyst should pay attention to when displaying or printing out data such as analysis results of multiple samples and multiple components.
  • Analysis result output processing device that can efficiently check data and graphs, and make accurate judgments and verifications based on such information, and an analysis result output processing program that runs on a computer There is to do.
  • An analysis result output processing apparatus which has been made to solve the above problems, processes data including quantitative results based on analysis results obtained by analyzing a large number of compounds for a large number of samples.
  • An analysis result output processing device for outputting, a) Information for identifying a sample and information for identifying a compound are arranged in a row direction and a column direction, respectively, and at least a part of data obtained for a combination of one sample and one compound A table creation unit for creating a two-dimensional table by assigning to a cell; b) A narrowing execution unit for determining data assigned to each cell of the table according to a preset narrowing condition, and identifying a cell to which data satisfying the narrowing condition is assigned; c) Numerical values based on data assigned to cells not specified by the narrowing execution unit in the table, or numerical values based on data assigned to cells specified by the narrowing execution unit.
  • a narrowed reflection display processing unit that outputs a table that is the same matrix arrangement as the table, which is displayed in a thin display compared to a display using characters or graphs, for display on a screen of the display unit or printing. It is characterized by having.
  • an analysis result output processing program for operating a computer for output, a) Information for identifying a sample and information for identifying a compound are arranged in a row direction and a column direction, respectively, and at least a part of data obtained for a combination of one sample and one compound A table creation step for creating a two-dimensional table by assigning it to a cell; b) A filtering execution step of determining data assigned to each cell of the table according to a preset filtering condition, and specifying a cell to which data satisfying the filtering condition is assigned; c) Numerical values based on the data assigned to the cells not specified by the narrowing execution step in the table, or numerical values based on the data assigned to the cells specified by the narrowing execution step.
  • a narrowed reflection display processing step for outputting a table having the same matrix arrangement as the table, which is displayed in a thin display as compared with the display by characters or graphs, for displaying on the screen of the display unit or for printing, It is characterized by having a computer execute.
  • analyzer for analyzing a large number of compounds for each of a large number of samples, that is, for analyzing a multi-sample / multi-component
  • a typical example is the liquid chromatograph described above. Gas chromatograph, liquid chromatograph mass spectrometer, gas chromatograph mass spectrometer and the like.
  • the table creation unit is, for example, a quantification obtained for each compound for a large number of samples.
  • a table is created by assigning values (concentration values, peak area values, etc.) to cells corresponding to combinations of samples and compounds.
  • this table is not necessarily displayed and may be created virtually in the course of data processing.
  • the refinement execution unit stores, for example, refinement conditions set in advance by an analyst and parameters related thereto, determines data assigned to each cell of the table according to the refinement conditions, and satisfies the refinement condition. Identify the cell to which data is assigned. For example, when a compound that exceeds the regulation value is important as in the above-described residual agricultural chemical test, it may be set as a narrowing condition to exceed a predetermined threshold.
  • the refinement reflection display processing unit is identified by the refinement execution unit, such as a numerical value or graph display such as a quantitative value assigned to a cell that has not been identified by the refinement execution unit, that is, that has not remained in the refinement.
  • the “thin display” here is a translucent display that usually shows the background transparent on the screen of the display unit of the computer.
  • the narrowing-down condition is a threshold value for determining the magnitude of the numerical value
  • the narrowing-down reflection display processing unit is assigned to the cell specified by the narrowing-down execution unit.
  • the threshold value used for the numerical value determination can be confirmed at a glance, for example, it can be easily understood how much the quantitative value exceeds the threshold value. It is also easy to find a threshold setting error.
  • the narrowed reflection display processing unit includes a first table that displays a numerical value based on data assigned to each cell, and a graph based on the data assigned to each cell.
  • the display of the graph in the cell not specified by the narrowing down execution unit is lighter than the display of the graph in the specified cell at least in the second table. It is good also as composition to do.
  • the chromatogram in which the peak used when calculating the quantitative value exceeding the reference threshold is observed is clearly shown in the second table, and the other chromatograms are displayed lightly. That is, for example, only the chromatograms that require confirmation that the peak shape is appropriate or that other peaks do not overlap are clearly shown, and the chromatogram shows which sample and which compound Since it can be seen at a glance whether it corresponds to the combination of the above, the analyst can efficiently proceed with the confirmation work.
  • the narrowing reflection display processing unit is configured to output all cells in one or a plurality of continuous row directions or one or a plurality of continuous columns in an output table.
  • the narrowing reflection display processing unit is configured to output all cells in one or a plurality of continuous row directions or one or a plurality of continuous columns in an output table.
  • the number is very small compared to the total number of measurement target compounds. Therefore, when the analysis result output processing apparatus according to the present invention is used for such inspection, the numerical values and graphs in most cells in the displayed table are displayed lightly. According to the above configuration, in such a case, since many rows and columns are hidden, the displayed table becomes small, and a quantitative value exceeding the threshold value and a combination of a sample and a compound that can obtain the quantitative value can be easily obtained. Can be found.
  • the analysis results of multiple samples and multiple components are narrowed down to, for example, combinations of a sample and a compound whose quantitative value exceeds a reference value.
  • the relationship between the rows and columns of the displayed table is maintained by the narrowing down, and the quantitative results etc. removed by the narrowing down can be clearly and easily discriminated from the quantitative results remaining in the narrowing down. . Therefore, the analyst can easily grasp the numerical values and graphs to be analyzed or noticed, or the combination of the sample and the compound, and can improve the efficiency of the analysis work of the quantitative results. In addition, mistakes in judgment and evaluation in such analysis work are less likely to occur.
  • FIG. 1 is a schematic configuration diagram of an embodiment of a GC-MS analysis system using an analysis result output processing apparatus according to the present invention.
  • the figure which shows the frame and item of the numerical information table and graph drawing table which are displayed in the GC-MS analysis system of a present Example.
  • Explanatory drawing of the creation and display process of a numerical information table in the GC-MS analysis system of a present Example Explanatory drawing of the creation and display process of the numerical information table in the GC-MS analysis system of a present Example.
  • Explanatory drawing of creation of a graph drawing table and a display process in the GC-MS analysis system of a present Example Explanatory drawing of creation of a graph drawing table and a display process in the GC-MS analysis system of a present Example.
  • Explanatory drawing of creation of a graph drawing table and a display process in the GC-MS analysis system of a present Example Explanatory drawing of creation of a graph drawing table and a display process in the GC-MS analysis system of a present
  • Explanatory drawing of creation of a graph drawing table and a display process in the GC-MS analysis system of a present Example Explanatory drawing of the printing output process of the numerical information table in the GC-MS analysis system of a present Example. Explanatory drawing of the printing output process of the numerical information table in the GC-MS analysis system of a present Example. Explanatory drawing of the printing output process of the numerical information table in the GC-MS analysis system of a present Example. Explanatory drawing of the printing output process of the numerical information table in the GC-MS analysis system of a present Example.
  • FIG. 1 is a schematic configuration diagram of a GC-MS analysis system according to this embodiment.
  • This GC-MS analysis system includes a GC-MS measurement unit 1 to which a gas chromatograph (GC) for temporally separating a compound contained in a sample (specimen) and a mass spectrometer (MS) for detecting the compound are connected.
  • a data processing unit 2 for processing data obtained by the GC-MS measuring unit 1, an input unit 3 for an analyst to input parameters and the like necessary for processing in the data processing unit 2, and a data processing unit 2
  • a display unit 4 on which the processing result is displayed and a printing unit 5 on which the processing result in the data processing unit 2 is printed out are provided.
  • the data processing unit 2 includes a data storage unit 20, a quantitative analysis unit 21, a numerical information table creation unit 22, a graph drawing table creation unit 23, a narrowing condition storage unit 24, a narrowing determination unit 25, a table display processing unit 26, and a table output process.
  • a functional block such as a unit 27 is included.
  • the substance of the data processing unit 2 is a personal computer (or a higher-performance workstation), and is a function embodied by executing a dedicated processing program installed in advance in the computer.
  • the characteristic operation in the GC-MS analysis system of the present embodiment is described by taking as an example a case where quantitative analysis of a plurality of predetermined compounds is performed, such as a pesticide residue test according to a positive list. To do.
  • a quantitative analysis since the compound to be measured in the GC-MS measurement unit 1 is known, a predetermined time range near the time when the known compound is introduced into the mass spectrometer, that is, around the retention time of the compound.
  • the analysis conditions in the mass spectrometer are set so as to perform SIM measurement at a mass-to-charge ratio m / z corresponding to the compound.
  • the MRM in the combination (MRM transition) of the characteristic mass-to-charge ratio of the precursor ion and the mass-to-charge ratio of the product ion corresponding to the compound Analysis conditions are set to perform measurement. Therefore, when one sample is measured in the GC-MS measurement unit 1, the temporal change in ion intensity at a predetermined mass-to-charge ratio (or a predetermined MRM transition) over a predetermined time range for each of a plurality of measurement target compounds. Is obtained.
  • This measurement data is stored in the data storage unit 20. At this time, information related to analysis such as the sample name given to the sample and the name of the measurement target compound is also stored.
  • the quantitative analysis unit 21 calculates a quantitative value (concentration value) based on the measurement data stored in the data storage unit 20. Specifically, based on the measurement data, a mass chromatogram is created for each measurement target compound, a peak appearing in the vicinity of the retention time corresponding to the compound is detected, and an area value (or height value) is obtained. Then, a quantitative value is derived from the area value with reference to a calibration curve prepared in advance based on the result of measuring the standard product. Information such as the quantitative value calculated in this way, the peak area value and height value obtained in the process, and the retention time obtained from the detected peak top position is associated with the measurement data or the measurement data. Store in the same file or folder.
  • the analysis processing by the quantitative analysis unit 21 may be executed in batch after the measurement for all the samples is completed, or may be executed sequentially during measurement of the samples.
  • a large amount of measurement data, quantitative results, etc. are stored in the data storage unit 20.
  • an analyst confirms and evaluates such quantitative results, for example, a compound whose quantitative value deviates from a reference value is quickly found, and whether or not the chromatogram peak obtained for the compound is appropriate.
  • the numerical information table creation unit 22 is based on the data read from the data storage unit 20 as shown in FIG. As shown, a matrix-like table is created with the sample information in the horizontal direction and the compound information in the vertical direction, and data such as quantitative values for the combination of the sample and the compound is assigned to each cell.
  • the table display processing unit 26 displays such a matrix-like numerical information table on the screen of the display unit 4.
  • sample-specific data and information for example, sample name, sample type (for example, standard sample, unknown sample, etc.), measurement date and time, measurer, etc. are set as data associated with the sample (having sample attributes).
  • compound-specific data and information such as compound name, retention time, quantitative ions (mass-to-charge ratio of ions used for quantification), peak area value (or height value), quantitative value (concentration value), etc.
  • Data associated with a compound (having compound attributes) is stored.
  • the data for one compound in one sample is a mixture of data having a compound attribute and data having a sample attribute.
  • FIG. Va n 1, Va n 2 data having the attribute of the sample, Vb m 1, Vb m 2 is data having an attribute of the compound.
  • four pieces of data are assigned to each cell of the numerical information table.
  • the matrix-like table shown in FIG. 3 (a) can be displayed separately for each sample and each compound as shown in FIG. 3 (b). Will be associated with a table for each compound.
  • FIG. 3B is an example of a table for each compound displayed when the top row (sample: Prop A1) of the table for each sample is designated.
  • the analyst can specify the sample name on the table for each sample, and examine the quantitative value of each compound in the table for each compound displayed correspondingly. Note that not all data assigned to each cell in the table is displayed in the table, but only arbitrary items designated by the analyst, for example, quantitative values can be displayed.
  • the analyst When the analyst wants to confirm only data that satisfies a specific condition, the analyst inputs and sets a narrowing condition for identifying the item to be confirmed from others from the input unit 3. For example, when it is desired to confirm that the quantitative value exceeds the reference value, the condition may be set so that the quantitative value exceeding the reference value remains in the narrowing down.
  • a different reference value can be set for each compound, or a reference value can be set for each sample.
  • narrowing conditions for other numerical information such as peak area values, and furthermore, narrowing conditions can be set for character information such as sample names and compound names. A character string included in the sample name can be excluded by narrowing down, or conversely, can be left narrowed down.
  • the input narrowing condition is stored in the narrowing condition storage unit 24.
  • a narrowing condition is set such that the compound: Prop B3 data: Vb 3 1 in the sample: Prop A1 is excluded by narrowing.
  • the refinement determination unit 25 determines each numerical value according to the refinement condition. In this case, as shown in FIG. 4A, only the data indicated by x in the table for each compound is an exclusion target based on the determination result.
  • the table display processing unit 26 determines that the data of the compound: Prop B3 in the sample: Prop A1 is not required to be displayed, and the top row (that is, the sample: Prop A1) in the table for each sample. Is selected, the display of the compound: Prop B3 line is deleted from the table for each compound (see FIG. 4B1).
  • the graph drawing table creation unit 23 creates a graph drawing table in which reduced images of the obtained chromatograms are arranged so as to have the same matrix arrangement as the matrix-like table created in the numerical information table creation unit 22. For example, when the numerical information table has 3 rows and 3 columns as shown in FIG. 3A, the graph drawing table also has 3 rows and 3 columns.
  • FIG. 5 is a schematic diagram when the numerical information table and the graph drawing table created in this way are displayed on the screen of the display unit 4.
  • FIG. 6 shows compound: Prop B1 for sample: Prop A1, compound: Prop B1 and Prop B2 for sample: Prop A2, and compound: Prop B3 for sample: Prop A3. It is a graph drawing table displayed when remaining by narrowing down. In this way, it is possible to grasp at a glance the graph remaining in the refinement and the graph excluded by the refinement, and it is possible to easily recognize which combination of the sample and the compound remains after the refinement.
  • FIG. 7 is an example of a graph drawing table display when the number of compounds to be measured per sample is larger (in this example, 6).
  • the number of compounds to be measured per sample is larger (in this example, 6).
  • two of the compounds: Prop B4 and Prop B5 are excluded by narrowing down all three samples, and the graph is displayed in a light color.
  • the analyst does not need to confirm two lines corresponding to the compounds: Prop B4 and Prop B5 on the graph drawing table. Therefore, as shown in FIG. 7B, instead of displaying these lines, a “+/ ⁇ ” button may be provided to indicate that these lines are not displayed and to switch between non-display / display. .
  • a “+/ ⁇ ” button may be provided to indicate that these lines are not displayed and to switch between non-display / display. .
  • the “+/ ⁇ ” button is displayed as “+”, and this display allows the analyst to recognize that there is a hidden line although the number of lines is unknown. it can.
  • the “+/ ⁇ ” button is clicked with a pointing device such as a mouse, the display is switched as shown in FIG. 7A, and all lines are displayed. .
  • one or more rows are hidden in units of rows, but similarly, one or more columns can be hidden in columns.
  • the analyst when displaying on the screen of the display unit 4, the analyst needs to efficiently check only the data remaining in the narrowing down. Therefore, as described above, the data excluded by the narrowing down is not displayed.
  • the data was displayed or displayed in a light display color with poor clarity, but if the quantitative results were printed out to create a report, the data excluded by filtering was also sufficient. It is preferable to output such that it is printed in a visually recognizable format. Therefore, in the system of this embodiment, the table output processing unit 27 performs processing different from that of the table display processing unit 26.
  • the threshold value for determining the quantitative value is 100, and those whose quantitative value is 100 or more are out of the reference value. That is, what should be noted is an item whose quantitative value is 100 or more.
  • the quantitative value that is less than the threshold is not indicated but only the character “ ⁇ 100” is shown.
  • the numerical value is shown about the quantitative value more than a threshold value.
  • the threshold value itself can be indicated by displaying “ ⁇ 100” for the quantitative value less than the threshold.
  • the narrowing conditions at the time of print output may be set separately from the narrowing conditions at the time of screen display, so that more flexible print output may be possible.
  • FIG. 9 is an example of print output when the threshold value for narrowing down is set in two stages.
  • FIG. 10 is an example in which the threshold value is shown in parentheses () in addition to FIG. 9.
  • the threshold value is divided into two stages of a limit value and a caution value that does not reach the limit value but requires attention, and “L” is added after the value of the quantitative value that the quantitative value exceeds the limit value. It is represented by letters, and the fact that the quantitative value exceeds the caution value is represented by the letter “R” added after the numerical value of the quantitative value.
  • the superscript display of the letters “L” and “R” represents the upper limit value
  • the subscript display represents the lower limit value.
  • the limit value and the caution value can be designated by the upper limit and the lower limit, respectively.
  • it may be expressed by a font difference indicating a quantitative value.
  • FIGS. 8 to 10 and the like may be used not only when printing, but also when displaying a numerical information table on the screen of the display unit 4.
  • a method of displaying information excluded by narrowing down in a light color as shown in FIG. 6 may be used when displaying the numerical information table.
  • the present invention was obtained not only by GC-MS but also by various analyzers such as LC, GC, LC-MS, and others. Obviously, it can be applied to data processing. In particular, when processing data obtained from multi-analyte multi-component analysis, numerical information such as quantitative values for a specific combination of a sample and a compound and a corresponding graph are visually confirmed.
  • the present invention is effective when it is desired to evaluate or evaluate.

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Abstract

Pendant l'affichage de résultats quantitatifs consolidé pour de multiples échantillons et de multiples constituants, une unité de traitement d'affichage de table (26) affiche, sur un écran d'affichage, une table d'informations numériques dans laquelle des valeurs quantitatives, ou analogue, sont disposées dans les cellules d'une table à deux dimensions dans laquelle des informations d'échantillon et des informations de constituant sont fournies dans la direction de rangée et la direction de colonne conjointement avec une table de traçage de graphes dans laquelle un chromatogramme de masse réduite est disposé à l'intérieur de la table dans des cellules qui ont la même disposition de rangées et de colonnes en tant que table d'informations numériques. Lorsqu'une condition de filtre est réglée pour déterminer des combinaisons de constituant et d'échantillon montrant des valeurs quantitatives dépassant une valeur de référence, une unité d'évaluation de filtrage (25) évalue les valeurs quantitatives de chaque cellule. Dans la table de traçage de graphes, l'unité de traitement d'affichage de table (26) affiche des chromatogrammes correspondant à des valeurs quantitatives éliminées par le filtrage dans une couleur plus claire (dispositif d'affichage semi-transparent) que d'autres chromatogrammes. Il en résulte que, tandis que les relations de rangées et de colonnes dans la table de traçage de graphes ne changent pas en tant que résultat du filtrage, il est non seulement plus facile de comprendre visuellement quels chromatogrammes sont restés après le filtrage mais aussi de comprendre des combinaisons de constituant et d'échantillon.
PCT/JP2015/068643 2015-06-29 2015-06-29 Dispositif de traitement de sortie de résultat d'analyse et programme de traitement de sortie de résultat d'analyse WO2017002156A1 (fr)

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JP2017525694A JP6447727B2 (ja) 2015-06-29 2015-06-29 分析結果出力処理装置及び分析結果出力処理用プログラム

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WO2018207228A1 (fr) * 2017-05-08 2018-11-15 株式会社島津製作所 Dispositif de traitement de données de spectroscopie de masse par chromatographe et programme de traitement de données de spectroscopie de masse par chromatographe
JP2019148455A (ja) * 2018-02-26 2019-09-05 株式会社島津製作所 測定データ処理方法、測定データ処理装置、及び測定データ処理用プログラム
CN111699393A (zh) * 2017-12-05 2020-09-22 株式会社岛津制作所 生物体试样分析系统
WO2020225864A1 (fr) * 2019-05-08 2020-11-12 株式会社島津製作所 Dispositif d'analyse

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JPWO2018207228A1 (ja) * 2017-05-08 2019-12-12 株式会社島津製作所 クロマトグラフ質量分析データ処理装置及びクロマトグラフ質量分析データ処理用プログラム
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CN113711031B (zh) * 2019-05-08 2024-01-23 株式会社岛津制作所 分析装置
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