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WO2018185889A1 - Dispositif de traitement de fichier de données de mesure et programme de traitement de fichier de données de mesure - Google Patents

Dispositif de traitement de fichier de données de mesure et programme de traitement de fichier de données de mesure Download PDF

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Publication number
WO2018185889A1
WO2018185889A1 PCT/JP2017/014276 JP2017014276W WO2018185889A1 WO 2018185889 A1 WO2018185889 A1 WO 2018185889A1 JP 2017014276 W JP2017014276 W JP 2017014276W WO 2018185889 A1 WO2018185889 A1 WO 2018185889A1
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Prior art keywords
measurement data
data file
partial
user
single measurement
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PCT/JP2017/014276
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English (en)
Japanese (ja)
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真二 杉本
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株式会社島津製作所
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Priority to PCT/JP2017/014276 priority Critical patent/WO2018185889A1/fr
Publication of WO2018185889A1 publication Critical patent/WO2018185889A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode

Definitions

  • the present invention relates to an apparatus and a program for processing a measurement data file containing data obtained by measuring a plurality of target compounds contained in a plurality of samples with an analyzer.
  • chromatographic mass spectrometers In order to identify and quantifying target compounds such as agricultural chemicals contained in samples such as foods, chromatographic mass spectrometers are widely used. As a method for identifying and quantifying a target compound in a sample using a chromatographic mass spectrometer, multiple reaction monitoring (MRM) measurement is known.
  • MRM multiple reaction monitoring
  • MRM measurement conditions including an MRM transition that is a set of a precursor ion generated from the target compound and a product ion generated by cleavage of the precursor ion are set in advance, and the MRM The intensity of product ions is measured under measurement conditions.
  • the MRM transition with the highest measurement sensitivity of product ions is used as the quantitative MRM transition
  • the MRM transition with the next highest measurement sensitivity of product ions is used as the confirmation MRM transition.
  • the analyst confirms the data in the measurement data file stored in the computer, and determines the peak area (or peak height) of the mass chromatogram of the quantitative MRM transition from the calibration curve obtained in advance by MRM measurement of the standard etc.
  • the target compound is quantified by comparison, and the ratio of the peak area (or peak height) of the mass chromatogram of the quantitative MRM transition to the peak area (or peak height) of the mass chromatogram of the confirmed MRM transition is determined in advance. It is confirmed (identified) that the peak of the mass chromatogram is that of the target compound by comparing with the ratio obtained by MRM measurement of a sample or the like (for example, Patent Document 1).
  • the analyst adds the result to the measurement data file and saves it in the computer.
  • target compounds such as agricultural chemicals contained in food samples
  • hundreds of types of target compounds may be analyzed (multi-component simultaneous analysis) for one sample.
  • a plurality of samples for example, 100
  • MRM measurement is sequentially performed on them to collect data. Since the number of MRM measurement data obtained in this way is the product of the number of samples and the target compound, a measurement data file containing tens of thousands of MRM measurement data is stored. While one analyst opens this measurement data file and performs the quantification and identification work for each target compound for each sample, the measurement data file is locked, and other analysts are in the measurement data file. Analysis of data cannot be performed. For this reason, there is a problem that one analyst has to analyze an enormous amount of data, and the burden on the analyst is large and the efficiency of the analysis is poor.
  • the problem to be solved by the present invention is to reduce the burden on the analyst involved in the analysis of data obtained by measuring a plurality of target compounds contained in a plurality of samples with an analyzer and increase the efficiency of the analysis.
  • a measurement data file processing apparatus and a measurement data file processing program are provided.
  • a measurement data file processing apparatus which has been made to solve the above problems, a) A plurality of single measurement data obtained by measuring a plurality of types of target compounds contained in each of a plurality of samples with an analyzer, each of which is data obtained by measuring one type of target compound contained in one sample.
  • a storage unit storing measurement data files for storing b) a classification form input receiving unit for allowing a user to input a form for classifying the plurality of single measurement data into a plurality of single measurement data groups each consisting of one to a plurality of single measurement data; c) classifying the plurality of single measurement data into a plurality of single measurement data groups based on the classification form, and for each of the plurality of single measurement data groups, single measurement included in the single measurement data group
  • a partial measurement data file creation unit for creating a partial measurement data file containing data; d) An integrated measurement data file creation unit that creates an integrated measurement data file by integrating a plurality of the partial measurement data files based on an instruction from a user.
  • the measurement data file processing apparatus is an apparatus for processing a measurement data file containing a plurality of single measurement data obtained by measuring a plurality of types of target compounds contained in each of a plurality of samples with an analyzer. It is.
  • the single measurement data is data of one type of target compound contained in one sample. For example, 100 single measurement data are obtained from the measurement results of 100 types of target compounds contained in one sample, and 10,000 single measurement data are obtained from 100 types of target compounds contained in each of 100 samples. It is done.
  • the single measurement data group is a set of one to a plurality of single measurement data.
  • the classification form input receiving unit causes the user to input how to classify a plurality of single measurement data.
  • the simplest way is to let the user input the number to classify a plurality of single measurement data (number of partial measurement data files to be created) and equalize the plurality of single measurement data by the number of classifications You can take the method of dividing into Further, a method of displaying a list of sample names or target compound names and allowing a user to classify a plurality of single measurement data by sample unit or target compound unit may be employed.
  • the partial measurement data file creation unit classifies a plurality of single measurement data in the input form and creates a partial measurement data file corresponding to each.
  • a plurality of partial measurement data files are created from one measurement data file, and each of them can be analyzed by another analyst.
  • the integrated measurement data file creation unit integrates them to create one integrated measurement data file.
  • the partial measurement data file creation unit attaches a rank between the partial measurement data files based on an input by a user when the partial measurement data file is created.
  • the single measurement data is generated when a plurality of partial measurement data files are integrated due to a problem when the partial measurement data file creation unit creates a partial measurement data file containing the single measurement data group after classification.
  • processing such as adopting single measurement data stored in one of the partial measurement data files can be performed based on the order between the partial measurement data files.
  • the input by the user may be an input of the order of the order itself, or an input of another information (for example, analysis difficulty level) may be used as it is as an order.
  • the measurement data processing apparatus is The storage unit stores in advance target compound information that is information associated with characteristics of a plurality of samples or a plurality of target compounds,
  • the classification form input receiving unit is preferably configured to present the target compound information to the user and allow the user to input a form for classifying the plurality of single measurement data.
  • a category of a sample or a target compound, an analysis difficulty level, or the like can be used.
  • single measurement data of samples or target compounds belonging to the same category can be aggregated into one partial measurement data file, or divided into multiple single measurement data groups according to analysis difficulty, and partial measurement containing these Data files can be sorted and analyzed according to the skill level of analysts.
  • the partial measurement data file creation unit may make the measurement data file a reference-only file when creating the plurality of partial measurement data files.
  • the partial measurement data file creation unit may set the measurement data file as one of the plurality of partial measurement data files.
  • the person in charge of analysis can use the measurement data file for analysis, and integrate the analysis results of other analysts.
  • a measurement data file processing program which has been made to solve the above problems, Accommodates multiple single measurement data, each of which is obtained by measuring multiple types of target compounds contained in multiple samples with an analyzer, each of which is a measurement of one type of target compound contained in one sample.
  • a computer that can access the storage unit that stores the measurement data file a) a classification form input receiving unit for allowing a user to input a form for classifying the plurality of single measurement data into a plurality of single measurement data groups including one to a plurality of single measurement data; b) classifying the plurality of single measurement data into a plurality of single measurement data groups based on the classification form, and for each of the plurality of single measurement data groups, single measurement data included in the single measurement data group; A partial measurement data file creation section for creating a stored partial measurement data file; c) It is characterized by operating as an integrated measurement data file creation unit for creating an integrated measurement data file by integrating a plurality of the partial measurement data files based on an instruction from a user.
  • the burden on the analyst involved in analyzing the data obtained by measuring a plurality of target compounds contained in a plurality of samples with the analyzer is reduced. Analysis efficiency can be increased.
  • the measurement data processing apparatus and the measurement data processing program of the present embodiment process a measurement data file containing data acquired by measurement using a liquid chromatograph mass spectrometer.
  • the liquid chromatograph mass spectrometer used for measurement in the present embodiment is roughly composed of a liquid chromatograph unit 1, a mass analyzer 2, and a control unit 4 that controls the operation thereof. This corresponds to the measurement data processing apparatus of this embodiment.
  • a liquid chromatograph mass spectrometry system in which a liquid chromatograph mass spectrometer and a measurement data file processing device are integrated is configured, and the measurement data file processing device controls operations such as measurement of the liquid chromatograph mass device.
  • the measurement data processing device can also be configured separately from the liquid chromatograph mass spectrometer.
  • the liquid chromatograph unit 1 includes a mobile phase container 10 in which a mobile phase is stored, a pump 11 that sucks the mobile phase and feeds it at a constant flow rate, and an injector 12 that injects a predetermined amount of sample liquid into the mobile phase. And a column 13 for separating various compounds contained in the sample solution in the time direction.
  • the liquid chromatograph unit 1 is connected to an autosampler 14 that introduces a plurality of liquid samples into the injector 12 one by one in a predetermined order and timing.
  • the mass analysis unit 2 includes a first intermediate vacuum whose degree of vacuum is increased stepwise between the ionization chamber 20 at approximately atmospheric pressure and the high-vacuum analysis chamber 23 evacuated by a vacuum pump (not shown).
  • a multi-stage differential exhaust system having a chamber 21 and a second intermediate vacuum chamber 22 is provided.
  • the ionization chamber 20 is provided with an electrospray ionization (ESI) probe 201 that sprays while applying a charge to the sample solution.
  • ESI electrospray ionization
  • the ionization chamber 20 and the first intermediate vacuum chamber 21 communicate with each other through a small heating capillary 202.
  • the first intermediate vacuum chamber 21 and the second intermediate vacuum chamber 22 are separated by a skimmer 212 having a small hole at the top, and ions are focused in the first intermediate vacuum chamber 21 and the second intermediate vacuum chamber 22, respectively.
  • a first ion guide 211 and a second ion guide 221 are provided for transporting to the subsequent stage.
  • the analysis chamber 23 sandwiches a collision cell 232 in which a multipole ion guide (q2) 233 is installed, and a front quadrupole mass filter (Q1) that separates ions according to the mass-to-charge ratio on the front side.
  • a collision-induced dissociation (CID) gas such as argon or nitrogen gas is appropriately supplied into the collision cell 232 in accordance with the measurement conditions.
  • the mass spectrometric section 2 can perform selected ion monitoring (SIM: Selected Ion Monitoring) measurement, MS / MS scan measurement (product ion scan measurement), multiple reaction monitoring (MRM: Multiple Reaction Monitoring) measurement, and the like.
  • SIM Selected Ion Monitoring
  • MS / MS scan measurement product ion scan measurement
  • MRM Multiple Reaction Monitoring
  • ions are not sorted by the front quadrupole mass filter (Q1) 231 (not functioning as a mass filter), and the mass-to-charge ratio of ions passing through the rear quadrupole mass filter (Q3) 234 is fixed. To detect ions.
  • both the front quadrupole mass filter (Q1) 231 and the rear quadrupole mass filter (Q3) 234 are caused to function as mass filters.
  • the front quadrupole mass filter (Q1) 231 only ions having a mass-to-charge ratio set as a precursor ion are allowed to pass through. Further, CID gas is supplied into the collision cell 232, and precursor ions are cleaved to generate product ions.
  • MS / MS scan measurement the mass-to-charge ratio of ions passing through the latter quadrupole mass filter (Q3) 234 is scanned, while in MRM measurement, the mass-to-charge ratio of ions passing through the latter quadrupole mass filter (Q3) 234 To detect product ions.
  • the control unit 4 includes a storage unit 41 and includes a classification form input reception unit 421, a partial measurement data file creation unit 422, and an integrated measurement data file creation unit 423 as functional blocks.
  • the entity of the control unit 4 is a personal computer, and the CPU of the personal computer functions as each of the above units by executing the measurement data file processing program 42 installed in advance in the computer.
  • An input unit 6 and a display unit 7 are connected to the control unit 4.
  • a sample table 411 and a compound table 412 are stored, and a measurement data file storage area 413 for storing a measurement data file is provided.
  • the sample table 411 associates information such as the sample name, the category to which the sample belongs, and the analysis difficulty level of the sample for each sample.
  • the compound table 412 includes, for each compound, the compound name, the category to which the compound belongs, the analysis difficulty level of the compound, measurement conditions (retention time, quantitative MRM transition and confirmation MRM transition of the compound, etc.), etc. Information is associated.
  • the measurement data file storage area 413 as shown in FIG. 4, data obtained by measuring a plurality of types (300 in this example) of target compounds contained in a plurality of samples (100 in this example) Is stored as a two-dimensional table with the target compound as one axis and the target compound as another axis. Note that data obtained by measuring one compound contained in one sample corresponds to the single measurement data, and the data shown in FIG. 4 includes 30,000 single measurement data.
  • the classification form input reception unit 421 When the user starts the measurement data file processing program by starting the measurement data file processing program or the like, the classification form input reception unit 421 first stores the measurement data file stored in the storage unit 41. The user selects a target to be processed (step S1). Subsequently, the classification form input receiving unit 421 displays a classification form input screen as shown in FIG. 6 on the screen of the display unit 7 (step S2). This screen displays four types of classification: “Classify by sample table”, “Classify by compound table”, “Classify evenly by sample”, and “Classify equally by compound”. The classification type input by the person is accepted. When the user selects and inputs “sort by sample table” or “sort by compound table”, the sample table 411 (see FIG. 2) or the compound table 412 (see FIG.
  • the classification input by the person is accepted.
  • an input screen for the number of classifications is then displayed, and the user inputs the number of classifications.
  • the 30,000 pieces of single measurement data are classified into the input numbers.
  • the single measurement data is classified into a plurality of pieces in the order of the single measurement data (that is, from the left or the top in FIG. 4). For example, when classifying into 10 samples by sample unit, in order from sample A, a single measurement data group (10 samples, 3,000 single measurement data corresponding to 300 types of target compounds) for each 10 samples Data group) and corresponding partial measurement data files are created.
  • the following processing will be described by taking as an example the case where the user selects “classify by compound table”.
  • the compound table shown in FIG. 4 is displayed on the screen.
  • the user can rearrange the list of compound tables for each item (compound name, category, difficulty level, etc.) of the compound table.
  • the list of compound tables can be rearranged in order of difficulty (analysis difficulty), and 300 types of compounds can be classified into a plurality (in this embodiment, 10) in descending order of analysis difficulty.
  • the partial measurement data file creation unit 422 selects a plurality of single measurement data (see FIG. 5) stored in the measurement data file according to the classification form. And a partial measurement data file corresponding to each is created (step S4).
  • 30,000 single measurement data in a compound unit are classified into 10 single measurement data groups in descending order of analysis difficulty of compound data (or in ascending order).
  • a partial measurement data file is created.
  • the ranks of the 10 partial measurement data files are assigned in descending order of analysis difficulty (step S5).
  • the user can also specify how to rank the partial measurement data file.
  • the measurement data file is set for reference only (not overwritten).
  • the partial measurement data file data obtained by adding columns for describing the analysis result of each single measurement data (quantitative value input column, compound identification result description column, etc.) to the single measurement data group is stored.
  • the 10 partial measurement data files created in this way are each subjected to analysis by an analyst, and each analyst identifies and quantifies each compound contained in each sample, and the result (quantitative) is displayed in the analysis result description column. Value, identification result) are described (step S6).
  • the integrated measurement data file creation unit 423 After the analysis of the single measurement data group by the analyst, when the user instructs the integration of the partial measurement data files via the input unit 6, the integrated measurement data file creation unit 423 has the single measurement data files stored in the ten partial measurement data files. The measurement data group and the analysis result are integrated to create an integrated measurement data file (step S7).
  • the integrated data file created here is obtained by adding an analysis result description column to the measurement data shown in FIG.
  • the integrated measurement data file creation unit 423 uses the sample name and compound name of the single measurement data and analysis results included in the created integrated measurement data file as the sample name and compound of the measurement data file (ie, the original single measurement data). Check whether there is any duplication or omission in single measurement data. When the single measurement data overlaps, the single measurement data and analysis results stored in the partial measurement data file with high rank are adopted, and the single measurement data and analysis results of the partial measurement data file with low rank are discarded. Usually, an analyst with a high degree of skill analyzes a single measurement data group of a compound with a high degree of difficulty. Therefore, the analysis result by an analyst with a high degree of skill is given priority. On the other hand, when the single measurement data is missing, the single measurement data is restored from the measurement data file and the display unit 7 displays that no analysis result has been input for the single measurement data.
  • the measurement data file processing apparatus and the measurement data file processing program of this embodiment are used, a plurality of partial analysis data files are created from one measurement data file, and each of them is analyzed by another analyst. It becomes possible to do. After the analyst analyzes each partial measurement data file, when the user instructs to integrate them, the integrated measurement data file creation unit 423 integrates them to create one integrated measurement data file. In this way, in this embodiment, since a plurality of partial measurement data files are created from one measurement data file, simultaneous analysis by multiple persons is possible, the burden on the analyst is reduced, and analysis efficiency is high. Become.
  • the sample form and compound table are displayed on the classification form input receiving unit 421, and the user can select a plurality of samples based on the analysis difficulty or category of the sample or compound. Since it is possible to classify single measurement data, it is classified into multiple single measurement data groups according to the type of sample or compound and the difficulty of analysis, and the partial measurement data file containing them is analyzed Depending on the situation, it can be sorted and analyzed.
  • the partial measurement data file creation unit 422 classifies into a plurality of single measurement data groups based on the form input by the user, creates a partial measurement data file corresponding to each group, and gives an order. At the same time, the measurement data file is set for reference only. Instead, for example, the partial measurement data file creation unit 422 sets the measurement data file with the analysis result input field as the partial measurement data file corresponding to the single measurement data group with the highest order. Can also be taken.
  • the integrated measurement data file creation unit 423 reflects the analysis result in the analysis result description column of the other partial measurement data file in this partial measurement data file (the measurement data file with the analysis result input column). To create an integrated measurement data file.
  • the above processing when single measurement data is duplicated is partial measurement data other than the partial measurement data file with the analysis result input field attached to the measurement data file. Applies only to files.
  • the partial measurement data file creation unit 422 creates the partial measurement data file by adding the analysis result input field to the plurality of single measurement data groups.
  • the analysis result is described separately from the plurality of single measurement data groups. It is also possible to create data consisting only of columns and associate this with a single measurement data group. In this case, a plurality of single measurement data groups may be set as reference-only data (that is, as data that cannot be overwritten).
  • the case where the measurement data file containing the data obtained by the MRM measurement using the liquid chromatograph mass spectrometer is processed has been described.
  • the same measurement data file processing apparatus and measurement data file processing program as those described above can be used when processing measurement data files containing acquired data or data obtained by various measurements using other analyzers. it can.
  • Sample table 412 ... Compound table 413 ... Measurement data file storage area 42 ... Measurement data file processing program 421 ... Classification form input acceptance unit 422 ... Partial measurement data file creation Part 423 ... Integrated measurement data Data file creation section 6 ... input section 7 ... display section

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Abstract

L'invention concerne un dispositif de traitement de fichier de données de mesure 4, caractérisé en ce qu'il comprend : une unité de stockage 41 qui conserve un fichier de données de mesure dans lequel une pluralité d'éléments de données de mesure unique sont stockés, qui sont obtenus par mesure, au moyen d'un dispositif d'analyse, d'une pluralité de types de composés cibles inclus dans une pluralité d'échantillons; une unité de réception d'entrée de format de classification 421 qui permet à un utilisateur d'entrer un format pour classifier la pluralité d'éléments de données de mesure unique en une pluralité de groupes de données de mesure; une unité de création de fichier de données de mesure partielle 422 qui classifie, sur la base du format de classification, la pluralité d'éléments de données de mesure unique en une pluralité de groupes de données de mesure unique et crée des fichiers de données de mesure partielle; et une unité de création de fichier de données de mesure intégrée 423 qui intègre, sur la base d'une commande par l'utilisateur, la pluralité de fichiers de données de mesure partielle pour créer un fichier de données de mesure intégré.
PCT/JP2017/014276 2017-04-05 2017-04-05 Dispositif de traitement de fichier de données de mesure et programme de traitement de fichier de données de mesure WO2018185889A1 (fr)

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Citations (2)

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Publication number Priority date Publication date Assignee Title
JPH113264A (ja) * 1997-06-13 1999-01-06 Hitachi Ltd ファイルの使用者優先順位設定によるファイル保護方式
JP2017020877A (ja) * 2015-07-10 2017-01-26 株式会社島津製作所 質量分析を用いた多成分一斉分析方法及び質量分析装置

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
JPH113264A (ja) * 1997-06-13 1999-01-06 Hitachi Ltd ファイルの使用者優先順位設定によるファイル保護方式
JP2017020877A (ja) * 2015-07-10 2017-01-26 株式会社島津製作所 質量分析を用いた多成分一斉分析方法及び質量分析装置

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