JP7131288B2 - Analyzer and analysis system - Google Patents

Description

The present invention relates to an analysis device and an analysis system.

An analysis system that manages and processes various data obtained by an analysis device is described in International Publication No. 2017/098599 (Patent Document 1). In the analysis system described in Patent Document 1, measurement data obtained by the analysis device and processing result data obtained by analyzing the measurement data are registered in a database constructed on a server connected to the analysis device. be done. In the analysis system, information on user's login/logout to the analysis device and various operations related to files is also registered in the database as operation log information. The operation log information includes details of the operation executed by the user, the date and time when the operation was performed, an ID for identifying the device on which the operation was performed, an ID for identifying the person in charge who performed the operation, and the like. included.

WO2017/098599

According to the analysis system described in Patent Document 1, for example, when submitting test results based on a data file stored in a database, operation log information related to this data file is extracted from the database. Can create an audit trail.

However, if an abnormality occurs in the analyzer during analysis, the internal state of the analyzer at the time of the abnormality cannot be known even by referring to the data files and operation log information accumulated in the database. It is feared that a great deal of labor will be required for anomaly analysis.

SUMMARY OF THE INVENTION The present invention has been made to solve such problems, and an object of the present invention is to provide an analysis system for managing and processing data collected by an analysis device, in which a user who manages and processes data is provided. It is to improve convenience.

According to one aspect of the present invention, an analysis device includes a device body that analyzes a sample, and an information processing device that controls the operation of the device body. The information processing device is configured to collect operation logs indicating internal operations of the device body. In the operation log, information indicating operation commands issued by the information processing apparatus and information indicating details of operations executed by the apparatus body in response to the operation instructions are associated one-to-one.

According to the analyzer, by collecting the operation log indicating the internal operation of the apparatus main body, it is possible to know the internal state of the analyzer based on the collected operation log. According to this, it is possible to grasp the internal state of the analyzer when, for example, an abnormality occurs, so that it is possible to efficiently analyze the abnormality. In addition, in the operation log, the information indicating the operation command and the information indicating the operation content in response to this operation command are associated one-to-one. can be easily collated, it becomes easy to detect an erroneous operation that violates the operation instruction. As a result, it is possible to improve convenience for the user who manages and processes data.

In the above analysis apparatus, preferably, in the action log, information indicating an action command is tagged to indicate that the information is related to the action command, and information indicating the content of the action is tagged to indicate that the information is related to the content of the action. attached.

According to this, it is possible to easily distinguish between the information indicating the action command and the information indicating the content of the action, so that the user's convenience can be improved.

Preferably, in the analysis device described above, the operation log further includes information indicating the purpose of the operation of the device main body. According to this, the user can easily recognize which phase of the operation the operation command and the operation content indicate.

Preferably, in the analysis device described above, the operation log further includes information indicating a result derived by the information processing device based on the operation of the device main body. According to this, the user can easily recognize the action content in response to the action instruction and the result based on this action content.

According to another aspect of the present invention, an analysis system includes the above analysis device and a server communicatively connected to the above analysis device. The analysis device is configured to send the collected operational logs to the server. The server has a storage unit for saving operation logs.

According to the above analysis system, the server can know the internal state of the analyzer based on the operation log stored in the storage unit, so that the operation of the analyzer can be efficiently analyzed.

In the analysis system described above, the analysis device is preferably configured to transmit an operation log to the server when an abnormality of the analysis device is detected. According to this, the operation log saved in the storage unit can be used to efficiently analyze the abnormality of the analyzer.

Preferably, in the analysis system, the analysis device is configured to periodically transmit the operation log to the server. Using the operation log saved in the storage unit, the presence or absence of an anomaly sign of the analyzer is diagnosed. According to this, it is possible to detect an anomaly sign of the analyzer using the operation log saved in the storage unit.

Preferably, in the above analysis system, the analysis device is configured to periodically transmit the operation log to the server. Using the operation log saved in the storage unit, calibration is performed to ensure the analysis accuracy of the analyzer. According to this, the operation log saved in the storage unit can be used to properly calibrate the analyzer.

According to the present invention, in an analysis system that manages and processes data collected by an analysis device, it is possible to improve convenience for users who manage and process data.

1 is a schematic diagram illustrating a configuration example of an analysis system according to this embodiment; FIG. FIG. 2 is a diagram schematically showing a configuration example of the analysis device shown in FIG. 1; 1 is a diagram schematically showing the configuration of an information processing device; FIG. It is a figure which shows the structure of a server roughly. 4 is a flowchart for explaining a processing procedure when executing automatic voltage adjustment; It is a figure which shows an example of a voltage adjustment execution setting screen. It is a figure which shows an example of an optimization result screen. It is a figure which shows an example of an optimization result screen. It is a figure which shows the structural example of a database. FIG. 4 is a diagram showing a first configuration example of an operation log; FIG. 11 is a diagram showing a second configuration example of an operation log; FIG. 11 is a diagram showing a third configuration example of an operation log; 4 is a flowchart for explaining a processing procedure when executing automatic voltage adjustment and abnormality predictive diagnosis; It is a figure which shows the measurement result of the relationship between a high frequency voltage value and signal strength. 15 is a diagram showing the relationship between the mass-to-charge ratio and the high-frequency voltage value based on the actual measurement results of FIG. 14; FIG. 4 is a flow chart for explaining a processing procedure when performing automatic voltage adjustment and calibration of the analyzer;

BEST MODE FOR CARRYING OUT THE INVENTION Below, embodiments of the present invention will be described in detail with reference to the drawings. In the following description, the same reference numerals are given to the same or corresponding parts in the drawings, and the description thereof will not be repeated in principle.

FIG. 1 is a schematic diagram illustrating a configuration example of an analysis system according to this embodiment.
Referring to FIG. 1, analysis system 100 according to the present embodiment is a system for analyzing a sample, and includes N units (N is an integer) of analysis devices AD1 to ADN, server 4, and database 5. .

Each of analyzers AD1-ADN is an apparatus for analyzing a sample. In the following description, the analyzers AD1 to ADN are also collectively referred to as analyzers AD. In this embodiment, a liquid chromatograph mass spectrometer (LC/MS) is exemplified as the analysis device AD.

The analyzer AD has an apparatus main body 1 and an information processing device 2 . The device main body 1 measures a sample. The information processing device 2 controls measurement in the device body 1 and performs quantitative analysis of data measured by the device body 1 . The information processing device 2 is connected to the Internet 3, which is a representative example of a communication network. As a result, the information processing devices 2 of the analysis devices AD1 to ADN are connected via the Internet 3 so as to be able to communicate with each other.

Furthermore, in analysis system 100 , server 4 is connected to Internet 3 . Therefore, the information processing device 2 of the analysis device AD can bidirectionally transmit and receive data to and from the server 4 via the Internet 3 .

The server 4 is mainly a server for managing the N analyzers AD in which the analysis system 100 is operated. The server 4 collects and manages information about the N analyzers AD by communicating with the N analyzers AD. The server 4 is, for example, a cloud server installed in a management center that manages the analysis system 100 .

A database 5 is connected to the server 4 . The database 5 is a storage unit for storing data exchanged between the server 4 and the analyzer AD. In the example of FIG. 1, the memory and the database 5 externally attached to the server 4 are used, but the server 4 may have a built-in storage unit. The database 5 corresponds to one embodiment of "storage".

FIG. 2 is a diagram schematically showing a configuration example of the analyzer AD shown in FIG.
Referring to FIG. 2, analyzer AD is a liquid chromatograph mass spectrometer (LC/MS). The device main body 1 includes a liquid chromatograph (LC) section 1A and a mass spectrometry (MS) section 1B.

The LC section 1A includes a mobile phase container 30, a liquid transfer pump 31, an injector 32, a column 33, a valve 34, and an adjustment sample introduction section . The liquid-sending pump 31 sucks the mobile phase stored in the mobile-phase container 30 and sends it to the column 33 through the injector 32 at a constant flow rate. When the sample is injected by the injector 32, the sample is introduced into the column 33 along with the flow of the mobile phase. eluted from the outlet of A valve 34 for channel switching is provided at the outlet of the column 33, and the eluate from the column 33 is introduced into the MS section 1B through the valve 34 during normal analysis.

An adjustment sample introduction section 35 is connected to the other side of the valve 34, and when automatic adjustment (auto-tuning) to be described later is executed, the valve 34 is switched and the sample liquid from the adjustment sample introduction section 35 is introduced into MS. Introduced in Part 1B. However, the method of introducing the sample for adjustment is not limited to this. Alternatively, a detour channel may be provided through which the mobile phase into which the adjustment sample is injected by the injector 32 bypasses the column 33, and the mobile phase may be introduced into the MS unit 1B through this detour channel.

The MS section 1B has a first intermediate vacuum chamber 43 and a second vacuum chamber 43 between an ionization chamber 40 having a substantially atmospheric pressure atmosphere and an analysis chamber 48 having a high vacuum atmosphere evacuated by a high-performance vacuum pump (not shown). It is a configuration of a multi-stage differential pumping system in which two intermediate vacuum chambers 46 are provided. The ionization chamber 40 and the first intermediate vacuum chamber 43 are communicated with each other by a solvent removal pipe 42 having a small diameter, and the first intermediate vacuum chamber 43 and the second intermediate vacuum chamber 46 are connected at the top of the skimmer 45. It communicates through a very small diameter passage hole (orifice).

In the MS section 1B, the eluate containing the sample components is sprayed into the ionization chamber 40 which is in a substantially atmospheric pressure atmosphere while being charged in the electrospray section 41, thereby ionizing the sample components. Note that ionization may be performed using other atmospheric pressure ionization methods such as the atmospheric pressure chemical ionization method, instead of the electrospray ionization method. Ions generated in the ionization chamber 40 and fine droplets in which the solvent has not yet completely evaporated are drawn into the desolvation pipe 42 by the differential pressure, and while passing through the heated desolvation pipe 42, further fine liquid droplets are formed. Evaporation of the solvent from the droplets proceeds and ions are generated.

In the first intermediate vacuum chamber 43, there is a first ion guide 44 in which a plurality of four electrode plates surrounding the ion optical axis C in a plane perpendicular to the ion optical axis C are arranged in the direction of the ion optical axis C. is provided. Ions are focused by this first ion guide 44, pass through the orifice, and enter the second intermediate vacuum chamber 46. FIG. A second ion guide 47 consisting of eight rod electrodes arranged so as to surround the ion optical axis C is provided in the second intermediate vacuum chamber 46 . sent to. In the analysis chamber 48, a quadrupole mass filter 50 consisting of four rod electrodes and a pre-rod electrode 49 consisting of four short rod electrodes in the direction of the ion optical axis C and located in front of the filter 50 are arranged. . Only ions having a specific mass-to-charge ratio among various ions pass through the quadrupole mass filter 50 and reach the ion detector 51 .

The information processing device 2 is mainly composed of a CPU (Central Processing Unit), which is an arithmetic processing unit. The information processing device 2 can use, for example, a personal computer. The information processing device 2 has a data processing section 60 , an analysis control section 62 and a central control section 64 . A signal detected by the ion detector 51 is input to the data processing unit 60, and various data processing such as creation of mass spectrum, mass chromatogram, and total ion chromatogram is executed. The analysis control unit 62 controls the operation of each unit of the LC unit 1A and the MS unit 1B, including power supply units 52 to 56 described later, in order to perform LC/MS analysis based on instructions from the central control unit 64. do. The central control unit 64 is connected to the input unit 22 and the display 24 as a user interface. The central control unit 64 outputs various commands for analysis to the analysis control unit 62 or the data processing unit 60 in response to the operator's operation through the input unit 22 . Also, the central control unit 64 outputs analysis results such as mass spectra to the display 24 . In the information processing apparatus 2, most of the central control unit 64, the analysis control unit 62 and the data processing unit 60 can be realized by a personal computer loaded with predetermined control/processing software.

A voltage V5 obtained by adding a predetermined DC bias voltage to a voltage obtained by superimposing a high frequency voltage and a DC voltage is applied to each rod electrode of the quadrupole mass filter 50 from the fifth power supply unit 56 . The mass-to-charge ratio that can pass through is determined according to the high-frequency voltage and the DC voltage.

A predetermined DC bias voltage V1 is applied to the desolvation tube 42 from the first power supply section 52 . A voltage V2 obtained by adding a DC bias voltage to a predetermined high frequency voltage is applied to the first ion guide 44 from the second power supply unit 53 . A voltage V3 obtained by adding a DC bias voltage to a predetermined high frequency voltage is applied to the second ion guide 47 from the third power supply unit 54 . Further, to the pre-rod electrode 49, a voltage V4 obtained by adding a predetermined DC bias voltage to a voltage obtained by superimposing a high-frequency voltage and a DC voltage is applied from the fourth power supply unit 55. FIG. In practice, a DC bias voltage is also applied to the skimmer 45 and the like, but only typical ones are described here in order to avoid complication of description.

FIG. 3 is a diagram schematically showing the configuration of the information processing device 2. As shown in FIG.
Referring to FIG. 3, information processing apparatus 2 includes a CPU 10 for controlling the entire apparatus and a storage section for storing programs and data, and is configured to operate according to programs. The storage unit includes ROM (Read Only Memory) 12 , RAM (Random Access Memory) 14 and HDD (Hard Disk Drive) 18 .

The ROM 12 can store programs executed by the CPU 10 . The RAM 14 can temporarily store data used during program execution in the CPU 10, and can function as a temporary data memory used as a work area. The HDD 18 is a non-volatile storage device, and can store information generated by the information processing device 2 such as measurement data by the device main body 1 and analysis results by the information processing device 2 . In addition to the HDD 18 or instead of the HDD 18, a semiconductor memory device such as a flash memory may be employed.

The information processing device 2 further includes a communication interface 20 , an I/O (Input/Output) interface 16 , an input section 22 and a display 24 . The communication interface 20 is an interface for the information processing device 2 to communicate with external devices including the device body 1 and the server 4 .

The I/O interface 16 is an interface for input to the information processing device 2 or output from the information processing device 2 . As shown in FIG. 3, I/O interface 16 is connected to input 22 and display 24 .

The input unit 22 receives input including instructions to the information processing device 2 from the subject. The input unit 22 includes a keyboard, a mouse, a touch panel integrated with the display screen of the display 24, and the like, and receives sample measurement conditions and the like.

The display 24 can display, for example, a measurement condition input screen and measurement data by the device main body 1 when setting the measurement conditions.

FIG. 4 is a diagram schematically showing the configuration of the server 4. As shown in FIG.
Referring to FIG. 4, server 4 includes a CPU 68 for controlling the entire device and a storage section for storing programs and data, and is configured to operate according to programs. The storage unit includes ROM 72 , RAM 74 , HDD 78 and database 5 .

The ROM 72 can store programs executed by the CPU 68 . The RAM 74 can temporarily store data used during program execution in the CPU 68, and can function as a temporary data memory used as a work area. The HDD 78 and the database 5 are nonvolatile storage devices, and can store information transmitted from the information processing device 2 .

Information processing device 2 further includes communication interface 75 and I/O interface 76 . The communication interface 75 is an interface for the server 4 to communicate with external devices including the information processing device 2 .

I/O interface 76 is an interface for input to or output from server 4 . I/O interface 76 is connected to database 5 . The database 5 is a memory for accumulating data transmitted and received between the server 4 and the information processing device 2 .

The server 4 can be configured to have functions equivalent to those of a general computer. Server 4 may further include a display unit and an input unit.

<Automatic adjustment function>
Referring to FIG. 2 again, the liquid chromatograph mass spectrometer, which is the analyzer AD, has many parameters for calibrating the mass-to-charge ratio and adjusting the mass resolution and analytical sensitivity. The parameters include voltages applied to each of the ionization interface, ion guide, quadrupole mass filter 50, ion trap and ion detector 51, and the like.

Calibration of the mass-to-charge ratio and adjustment of the instrument generally involves obtaining a mass spectrum by performing mass spectrometry on a standard sample with known components and concentrations, while ensuring that the peaks appearing in the spectrum are positioned appropriately. In addition, various parameters are adjusted to optimum values so that the peak intensity is as high as possible and the half-value width is as narrow as possible. In recent years, many apparatuses are provided with an automatic adjustment function (auto-tuning) for automatically adjusting such various parameters. For example, by performing automatic adjustment periodically, such as once a month, it is possible to maintain high levels of mass resolution and analytical sensitivity at all times.

Here, in order to achieve high mass resolution and analytical sensitivity in the liquid chromatograph mass spectrometer, among the ions generated in the ionization chamber 40 (or the desolvation tube 42, the first intermediate vacuum chamber 43), It is necessary that the ions to be analyzed are introduced into the quadrupole mass filter 50 with as high an efficiency as possible. For this purpose, it is necessary to maximize the ion passage efficiency in each of the ion transport optical elements described above.

As an example, focusing on the transport efficiency of ions from the ionization chamber 40 to the second intermediate vacuum chamber 46, in order to maximize the transport efficiency of the ions, It is important to appropriately set the DC bias voltage V1 applied to and the DC bias voltage V2 applied from the second power supply unit 53 to the second ion guide 47 according to the mass-to-charge ratio of passing ions. . Therefore, as part of the automatic adjustment function, automatic voltage adjustment is performed to automatically adjust the voltage applied to each location. The operation of the analyzer AD when performing automatic voltage adjustment will be described below.

FIG. 5 is a flowchart for explaining a processing procedure when executing automatic voltage adjustment.

Referring to FIG. 5, first, in step S01, the operator performs a predetermined operation using the input unit 22 to set analysis conditions for SIM (selective ion monitoring) measurement and voltage adjustment execution conditions. SIM measurement analysis conditions include, for example, one or more mass-to-charge ratios (m/z values) to be subjected to SIM measurement, the temperature of each part of the device, and the like.

In order to set the voltage adjustment execution condition, the operator performs a predetermined operation on the input unit 22 to display the setting screen 70 shown in FIG. The operator uses the input unit 22 to set the type of voltage optimization target (ion transport optical system), the voltage value adjustment range and voltage step number, the type of data used to determine the optimum value, and the like. In the example of FIG. 6, the optimization target is the DC voltage applied to the Q array (first ion guide 44), the voltage value adjustment range is 0 to 80 [V], and the number of voltage steps is 5. Yes, use the height or area of the chromatogram peak to calculate the optimal value.

After setting the necessary conditions and parameters on the setting screen 70 of FIG. 6, when the operator clicks the "start" button 71, the central control unit 64 performs a voltage adjustment operation for voltage optimization in step S02. Start. First, in step S03, an analysis method file for executing analysis is created based on the various conditions and parameters set in step S01. Next, in step S04, the analysis control section 62 performs actual measurement according to the created analysis method file.

Here, it is assumed that the DC voltage applied to the second ion guide 47 is changed in steps of 10 [V] within the range of 0 to 50 [V]. Assume that there are three m/z values M1, M2, and M3 for SIM measurement.

In this case, first, m/z=M1 is changed in the order of V1=0, 10, 20, 30, 40, 50 [V], and the adjustment sample prepared in the adjustment sample introduction part 35 is measured. to run. Alternatively, while the applied voltage is fixed at V1=0, m/z is changed in the order of M1, M2, and M3 to perform measurement, and after the measurement is completed, V1 is changed to 10 [V] and similar Measurements may be repeated. In any case, the same adjustment sample may be measured for all combinations of m/z values and applied voltages that have been set.

The adjustment sample is introduced into the MS section 1B from the adjustment sample introduction section 35 along with the mobile phase. The sample for adjustment is a standard sample prepared by the manufacturer of the analyzer AD or the like, and contains known components and known concentrations. However, the sample for adjustment may be a target sample prepared by the user of the analyzer AD (normally, a sample whose components are known).

During the measurement of the adjustment sample in step S04, the data processing unit 60 collects a log of the internal operation of the analyzer AD (hereinafter also referred to as "operation log") in step S05. The data processing unit 60 saves the collected operation log in the HDD 40 (see FIG. 2) inside the information processing apparatus 2 . In the specification of the present application, the "operation log" means information indicating an operation command issued inside the analysis device AD (information processing device 2) based on analysis conditions and/or operation conditions, and an actual log in response to this operation command. contains information indicating the contents of the operation performed by the analyzer AD (apparatus main body 1). The operation log saved in the HDD 40 can be used for abnormality analysis when an abnormality is detected during execution of automatic voltage adjustment, as will be described later.

Based on the detection signal from the ion detector 51, the data processing unit 60 creates a chromatogram showing the temporal change in signal intensity at the m/z value of interest. Next, the data processing unit 60 detects peaks in the created chromatogram and calculates, for example, peak areas. A chromatogram is generated for each m/z value and each applied voltage and the peak area values are obtained. In step S06, the data processing unit 60 compares the area values obtained when the applied voltage is changed with respect to the same m/z value, and determines the applied voltage that maximizes the area value as the optimum voltage value. can be determined.

Next, in step S<b>07 , the data processing unit 60 displays the optimization result screen 80 shown in FIG. 7 on the display screen of the display 24 . The optimization result screen 80 includes a graph 81 showing the relationship between signal strength and applied voltage. The vertical axis of the graph 81 is the peak area value, and the horizontal axis is the voltage value. The optimization results screen 80 also includes the chromatograms 82 obtained for each voltage value. Also included is an automatically determined optimal voltage value 83 (40.0 V in the example of FIG. 7).

In step S08, the operator checks the shape of the graph 81 and the chromatogram 82 on the optimization result screen 80 of FIG. 7, and determines whether or not the optimum voltage value 83 is appropriate. In the example of FIG. 7, the curve of the graph 81 peaks at the optimum voltage value of 40 V, and the area value spreads to the low voltage side and the high voltage side in a skirt shape. Also, the waveforms of the chromatogram 82 have no disturbance and are relatively similar regardless of the voltage value. From these facts, it can be determined that the optimum voltage value is appropriate. If the optimum voltage value is appropriate (when determined as YES in S08), when the operator clicks the "apply to method" button 84 included in the optimization result screen 80, the central control unit 64 performs this operation in step S09. is received, the optimum voltage value is determined, and this is reflected in the analysis conditions for SIM measurement.

On the other hand, if the optimum voltage value is not appropriate (NO determination in S08), the operator clicks the "non-apply" button 85 included in the optimization result screen 80. FIG. For example, as shown in FIG. 8, in the graph 81 shown on the optimization result screen 80, if there are two peaks, or if the peak area value deviates significantly from the assumed value for the standard sample If so, it is determined that the optimum voltage value is not appropriate. Alternatively, if the shape of the waveform is distorted in at least one of the chromatograms 82 obtained for each voltage value, it is determined that the optimum voltage value is not appropriate. If the optimum voltage value is not appropriate as described above, it can be detected that there is a possibility that some kind of abnormality has occurred inside the apparatus main body 1 .

The determination of whether or not the optimum voltage value is appropriate in step S08 may be performed by the information processing apparatus 2 instead of being performed by the operator. According to this, the burden on the operator can be reduced, and the determination can be made appropriately without being affected by the operator's experience, skill level, or the like. When the central control unit 64 determines that the optimum voltage value is appropriate, it automatically determines the optimum voltage value and reflects it in the analysis conditions for SIM measurement. On the other hand, when it is determined that the optimum voltage value is not appropriate, the central control unit 64 displays on the display 24 that the automatic voltage adjustment cannot be performed normally and that there is a possibility that an abnormality has occurred in the apparatus body 1. The operator can be notified using a display screen or other notification means.

If the optimum voltage value is not appropriate (NO determination in S08), in step S10, the central control unit 64 receives this operation and sends the operation log saved in the HDD 40 to the server 4 via the Internet 3. Send. Specifically, among the operation logs stored in HDD 40 , an operation log related to the current automatic voltage adjustment is extracted and transmitted to server 4 .

When the server 4 receives the operation log transmitted from the information processing device 2 of the analysis device AD via the Internet 3 in step S21, the server 4 stores the received operation log in the database 5. FIG. FIG. 9 shows a configuration example of the database 5. As shown in FIG. 9, database 5 stores operation logs of each of N analyzers AD1 to ADN (see FIG. 1) communicatively connected to server 4. FIG. The operation log is stored in one file for each analyzer AD. The operation log stored in each file indicates the internal operation of the analysis device AD when an abnormality is detected in the corresponding analysis device AD.

A management center that manages the analysis system 100 (for example, a support center operated by a device manufacturer of the analyzer AD) reads the operation log corresponding to the analyzer AD in which an abnormality has been detected from the database 5, and reads the read operation. The log can be used to analyze anomalies in the analyzer AD.

As described above, the operation log includes the operation command issued by the information processing device 2 and the information indicating the details of the operation actually performed by the device body 1 in response to this operation command. Therefore, by comparing the action command with the actual action content, an erroneous action violating the action command can be detected. Then, it is possible to identify the location of the malfunction that caused the malfunction, the content of the failure at the location of the malfunction, the cause of the failure, and the like from the content of the detected malfunction.

Returning to FIG. 5, in step S22, when the server 4 analyzes the abnormality of the analyzer AD using the operation log, the process proceeds to step S23 to transmit the result of the abnormality analysis to the analyzer AD via the Internet 3. It is transmitted to the information processing device 2 of AD. In step S<b>11 , when the information processing apparatus 2 receives the abnormality analysis result transmitted from the server 4 , the received abnormality analysis result is displayed on the display screen of the display 24 . The operator or the user of the analysis device AD can take measures such as requesting repair of the failure location or replacement of parts based on the result of the abnormality analysis. The server 4 corresponds to one embodiment of the "analyzer".

In the above-described embodiment, the configuration in which the operation log accumulated in the database 5 is used for abnormality analysis has been described. It is also possible to configure to perform

<Operation log>
Next, a configuration example of an operation log will be described with reference to FIGS. 10 to 12. FIG.

(Configuration example 1)
FIG. 10 is a diagram showing a first configuration example of an operation log. Referring to FIG. 10, in the first configuration example, the operation log has a text file format. The operation log includes an operation instruction (Command) issued by the information processing apparatus 2 and the operation content (Response) actually performed by the apparatus body 1 in response to this operation instruction. In the example of FIG. 7, character strings 200 and 202 indicating action commands and character strings 201 and 203 indicating action details are shown.

These strings are arranged in chronological order. Strings 200-203 have a message portion 110 expressed in multiple codes. In the example of FIG. 10, each of the multiple codes is composed of several digits. In the character strings 200 and 202 indicating action commands, each code represents information such as the output destination of the action command and the content of the action command. In the character strings 201 and 203 indicating the action content, each code represents information such as action content.

In the case of the voltage adjustment operation described above, the character strings 200 and 202 indicating the operation command include SIM measurement analysis conditions and voltage adjustment execution conditions (for example, information indicating the adjustment range of the voltage value and the number of voltage steps). The character strings 201 and 203 indicating the operation content include the actual applied voltage value, the detection signal of the ion detector 51, and the like. Strings 201, 203 also contain the chromatograms obtained for each voltage value.

As shown in FIG. 10, in the action log, a character string 200 indicating an action command and a character string 201 indicating action contents in response to the action command are associated one-to-one. Also, the character string 202 indicating the action command and the character string 204 indicating the content of the action in response to the action command are associated one-to-one. By storing a set of character strings indicating operation instructions and character strings indicating operation details in response to the operation instructions in this way, the person in charge of anomaly analysis can easily identify the operation instructions and the actual operation details. Since it can be collated, it becomes easy to detect an erroneous operation that violates the operation instruction. As a result, it becomes possible to efficiently perform abnormality analysis.

Note that the character strings 200 and 202 indicating action commands are tagged with a tag 101 of [Command], and the character strings 201 and 203 indicating actions are tagged with a tag 101 of [Response]. . By attaching a tag 101 to each character string, it is possible to easily distinguish between the information indicating the action command and the information indicating the content of the action.

(Configuration example 2)
FIG. 11 is a diagram showing a second configuration example of the operation log. Referring to FIG. 11, the second configuration example is different from the first configuration example shown in FIG. 7 in that a character string 204 indicating the purpose of the operation of the analyzer AD (apparatus main body 1) is added. .

In the automatic adjustment function of the analyzer AD, in addition to the voltage adjustment operation described above, the sensitivity adjustment and resolution adjustment of each section are sequentially performed according to a predetermined procedure. Therefore, even in the operation log, it is necessary to clarify which phase of the automatic adjustment function is being executed. In the example of FIG. 8, the character string 204 has a message portion 112 indicating the phase of automatic adjustment. According to this, it becomes clear for what kind of adjustment the analyzer AD is operated.

A tag 102 of [Phase] is attached to the beginning of the character string 204 . By attaching the tag 102, the person in charge of anomaly analysis can easily recognize that the character string indicates the phase.

(Configuration example 3)
FIG. 12 is a diagram showing a third configuration example of the operation log. Referring to FIG. 12, in the third configuration example, compared with the second configuration example shown in FIG. Column 205 is added.

In the voltage adjustment operation described above, the character string 205 includes information indicating the optimum voltage value set by the data processing unit 60 . Although illustration is omitted, the character string 205 can include information indicating various parameters set for each adjustment phase. According to this, the operation in response to the operation command and the parameters set based on this operation are shown in association with each other, so that the person in charge of abnormality analysis can perform the abnormality analysis more efficiently.

A tag 103 of [Result] is added to the beginning of the character string 205 . By attaching the tag 103, the person in charge of analysis can easily recognize that the character string indicates the result.

<Example of using operation log>
In the above-described embodiment, the configuration in which the operation log is used for abnormality analysis of the analyzer AD has been described. Operation logs can be utilized.

(1) Abnormality predictor diagnosis In the abnormality predictor diagnosis of the analyzer AD, the presence or absence of an abnormality predictor of the analyzer AD is diagnosed using the operation log collected during automatic adjustment. In the present embodiment, an operation log collected when the analyzer AD is operating normally is stored as a reference operation log, and based on the newly collected operation log and the reference operation log, , the presence or absence of a sign of abnormality in the analyzer AD.

FIG. 13 is a flowchart for explaining a processing procedure when executing automatic voltage adjustment and abnormality predictive diagnosis. The flowchart shown in FIG. 13 differs from the flowchart shown in FIG. 5 in that the timing of the operation log transmission process (step S10) and the server 4 executing the abnormality predictor diagnosis process (step S22A).

Specifically, referring to FIG. 13, analyzer AD executes the voltage adjustment operation by executing the same steps S01 to S06 as in FIG. are collected, and the collected operation logs are stored in the HDD 40 (see FIG. 2) inside the information processing apparatus 2 .

After determining the optimum voltage value in step S<b>06 , the analyzer AD proceeds to step S<b>10 and transmits the operation log stored in the HDD 40 to the server 4 via the Internet 3 . Specifically, among the operation logs stored in HDD 40 , an operation log related to the current automatic voltage adjustment is extracted and transmitted to server 4 .

In the flowchart of FIG. 13, the operation log at that time is transmitted to the server 4 each time the voltage adjustment operation is performed. According to this, when the automatic voltage adjustment is periodically executed, for example, once a month, the operation log is also periodically transmitted to the server 4 .

When the server 4 receives the operation log transmitted from the information processing device 2 of the analysis device AD via the Internet 3 in step S21, the received operation log is stored in the database 5 (see FIG. 9).

In step S22A, the management center that manages the analysis system 100 reads out the operation log corresponding to the analysis device AD from the database 5, and uses the read operation log to execute the abnormality predictive diagnosis of the analysis device AD. can. Specifically, the person in charge of analysis can compare the reference operation log stored in advance in the database 5 and the operation log newly acquired this time to the same operation command (Command) executed in response to the operation log. Compare the contents of the action (Response). If the operation contents match between these two operation logs, it can be diagnosed that there is no sign of abnormality.

On the other hand, if the operation contents do not match, it can be diagnosed that there is an anomaly sign. For example, the chromatogram shapes obtained for a certain voltage value are compared between the reference operation log and the current operation log. If a disturbance in the chromatogram waveform that is not seen in the reference operation log appears in the current operation log, it can be diagnosed that there is an anomaly sign.

Anomalies that occur in the analyzer AD are mainly caused by factors such as the sample adhering to the surface of each part due to repeated use of the analyzer AD, the surface being oxidized, and the physical arrangement being deviated. can occur due to By performing the above-described abnormality predictive diagnosis, an abnormality can be detected early at the symptom stage. Then, in step S23A, the server 4 notifies the user of the analysis device AD of the detection of the sign of abnormality, thereby recommending replacement of deteriorated parts. As a result, it is possible to prevent an abnormality from occurring in the analyzer AD. The server 4 corresponds to one embodiment of a "diagnostic unit".

In the above-described embodiment, a configuration for diagnosing the presence or absence of an anomaly sign based on the result of comparing a reference operation log stored in advance for one analyzer AD and a newly collected operation log will be described. However, by comparing a plurality of operation logs respectively collected in a plurality of analysis devices AD connected to the server 4, it is possible to diagnose the presence or absence of an anomaly sign.

(2) Assurance of Analysis Accuracy In the analysis accuracy assurance of the analyzer AD, the operation log collected during automatic adjustment is used to perform calibration for assuring the analysis accuracy of the analyzer AD.

FIG. 14 shows the relationship between the voltage value of the high-frequency voltage applied to the first ion guide 44 (see FIG. 2) and the signal intensity (here, normalized ion intensity) detected by the ion detector 51. is a diagram showing the results of actual measurements at the mass-to-charge ratio of . FIG. 15 is a diagram showing the relationship between the mass-to-charge ratio and the optimum voltage value (the voltage value that gives the maximum ion intensity) obtained based on the actual measurement results of FIG.

Referring to FIG. 14, the change in signal intensity with respect to the change in the voltage value of the high-frequency voltage shows a substantially mountain-shaped peak. It can be seen that the larger the ratio, the wider the area.

Also, from the results of FIG. 15, it can be seen that there is a proportional relationship between the mass-to-charge ratio and the optimum voltage value. In FIG. 15, the relationship between the mass-to-charge ratio and the optimum voltage value is approximated by a straight line. The relational expression representing the straight line shown in FIG. 15 can be initially calculated by the manufacturer of the analyzer AD based on the actual measurement results. A table showing the relationship between the mass-to-charge ratio and the optimum voltage value may be created instead of the data showing the relational expression.

However, for example, when the analysis device AD is disassembled and reassembled for the purpose of removing dirt from the first ion guide 44, or when the first ion guide 44 is replaced with a new one, the electrode plate The above relational expression may change due to a slight change in the arrangement of . For such a case, a process for newly obtaining the above relational expression is periodically executed. An operation log collected during automatic adjustment is used for this process.

Specifically, every time the voltage value of the high-frequency voltage applied to the first ion guide 44 changes, the data processing unit 60 acquires signal intensity data at a plurality of mass-to-charge ratios, and uses the acquired signal intensity data as The voltage value at which the signal intensity is maximized is calculated as the optimum voltage value. The data processing unit 60 collects the relationship between the mass-to-charge ratio and the optimum voltage value obtained based on the actual measurement results as an operation log and stores it in the HDD 40 . The information processing device 2 transmits the operation log stored in the HDD 40 to the server 4 via the Internet 3 .

When the server 4 receives the operation log transmitted from the information processing device 2 of the analysis device AD via the Internet 3, the received operation log is stored in the database 5 (see FIG. 9). The management center that manages the analysis system 100 reads the operation log corresponding to the analysis device AD from the database 5 and calculates the relational expression using this read operation log.

In calculating the relational expression, the server 4 determines whether or not the mass-to-charge ratio and the optimum voltage value included in the operation log have a proportional relationship. A plurality of measurement points indicating the relationship between the mass-to-charge ratio and the optimum voltage value may include measurement points that are greatly deviated from the straight line in FIG. As a factor for this, it is conceivable that the shape of the peak of the signal intensity shown in FIG. 14 was broken from the mountain shape, and the optimum voltage value was not detected correctly. If such measurement points are used, there is a concern that a correct relational expression cannot be obtained.

Therefore, the server 4 calculates the relational expression by excluding inappropriate measurement points from the plurality of measurement points obtained from the operation log. By doing so, a correct relational expression can be obtained, so that the analysis accuracy of the analyzer AD can be guaranteed.

FIG. 16 is a flow chart for explaining a processing procedure when executing automatic voltage adjustment and calibration of the analyzer. The flowchart shown in FIG. 16 differs from the flowchart shown in FIG. 5 in that the timing of the operation log transmission process (step S10) and the process of the server 4 creating the relational expression (or table) of the analyzer AD (step S22B) is executed.

Specifically, referring to FIG. 16, analyzer AD executes the voltage adjustment operation by executing the same steps S01 to S06 as in FIG. are collected, and the collected operation logs are stored in the HDD 40 (see FIG. 2) inside the information processing apparatus 2 .

After collecting the operation log and storing it in the HDD 40 in step S<b>05 , the analysis apparatus AD proceeds to step S<b>10 and transmits the operation log stored in the HDD 40 to the server 4 via the Internet 3 .

In the flowchart of FIG. 16, in step S22B, the analyzer AD is calibrated using the operation log transmitted each time the voltage adjustment operation is performed. Specifically, when the server 4 receives the operation log transmitted from the information processing device 2 of the analysis device AD via the Internet 3 in step S21, the server 4 stores the received operation log in the database 5 (Fig. 9).

In step S22B, the server 4 reads the operation log corresponding to the analyzer AD from the database 5, and uses this read operation log to create a relational expression or table indicating the relationship between the mass-to-charge ratio and the optimum voltage value. do. At this time, the server 4 calculates a relational expression or table by excluding inappropriate measurement points from the plurality of measurement points obtained from the operation log. Server 4 transmits the created relational expression or table to analysis device AD in step S23B. When the analysis device AD receives the relational expression or table in step S11B, it stores it in the HDD 40 .

In the present embodiment, a liquid chromatograph mass spectrometer has been exemplified as an analysis device, but the analysis device is a device that analyzes a sample even if it is not a liquid chromatograph mass spectrometer, It is possible to apply an analysis device having a function of exchanging data with a server.

It should be considered that the embodiments disclosed this time are illustrative in all respects and not restrictive. The scope of the present invention is indicated by the scope of the claims rather than the above description, and is intended to include all modifications within the meaning and range of equivalents of the scope of the claims.

1 device body, 2 information processing device, 3 Internet, 4 server, 5 database, 10, 68 CPU, 12, 72 ROM, 14, 74 RAM, 16, 76 I/O interface, 20, 75 communication interface, 22 input unit , 24 display, 30 mobile phase container, 31 liquid pump, 32 injector, 33 column, 34 valve, 35 adjustment sample introduction part, 40 ionization chamber, 42 desolvation tube, 44 first ion guide, 45 skimmer, 46 second second Intermediate vacuum chamber 47 Second ion guide 48 Analysis chamber 49 Pre-rod electrode 50 Mass filter 52 First power supply unit 53 Second power supply unit 54 Third power supply unit 55 Fourth power supply unit 56 Fifth power supply Section 60 Data Processing Section 62 Analysis Control Section 64 Central Control Section 70 Setting Screen 71, 84, 85 Buttons 80 Optimization Result Screen 81 Graph 82 Chromatogram 100 Analysis System 101, 102, 103 Tag, 110, 112 Message part, 200-205 String, AD, AD1-ADN Analyzer.

Claims (11)

a device body for analyzing a sample;
An information processing device that controls the operation of the device main body,
The information processing device is configured to collect operation logs indicating internal operations of the device main body,
The operation log contains information indicating an operation instruction issued by the information processing apparatus based on analysis conditions and/or operation conditions, and information indicating operation details executed by the apparatus main body in response to the operation instruction. are associated one-to-one ,
The analysis device , wherein the operation log further includes information indicating the purpose of the operation of the device main body . In the action log, the information indicating the action command is tagged to indicate that the information relates to the action command, and the information indicating the content of the action is tagged to indicate that the information relates to the content of the action. 2. The analytical device of claim 1, wherein 3. The analysis device according to claim 1, wherein said operation log further includes information indicating a result derived by said information processing device based on the operation of said device main body. a device body for analyzing a sample;
An information processing device that controls the operation of the device main body,
The information processing device is configured to collect operation logs indicating internal operations of the device main body,
The operation log contains information indicating an operation instruction issued by the information processing apparatus based on analysis conditions and/or operation conditions, and information indicating operation details executed by the apparatus main body in response to the operation instruction. are associated one-to-one,
The analysis device, wherein the operation log further includes information indicating a result derived by the information processing device based on the operation of the device main body. The analyzer according to any one of claims 1 to 4;
A server connected for communication with the analysis device,
The analysis device is configured to transmit the collected operation log to the server;
The analysis system, wherein the server has a storage unit for storing the operation log. The analysis device is configured to transmit to the server the operation log when an abnormality of the analysis device is detected,
6. The analysis system according to claim 5, wherein an abnormality analysis of said analysis device is performed using said operation log saved in said storage unit. The analysis device is configured to periodically transmit the operation log to the server;
6. The analysis system according to claim 5, wherein the operation log stored in the storage unit is used to diagnose whether or not there is an anomaly sign of the analysis device. The analysis device is configured to periodically transmit the operation log to the server;
6. The analysis system according to claim 5, wherein the operation log stored in the storage unit is used to perform calibration for ensuring analysis accuracy of the analysis device. an analyzer;
an analysis unit for executing abnormality analysis of the analysis device,
The analysis device is
a device body for analyzing a sample;
an information processing device that controls the operation of the device main body,
The information processing device is configured to collect operation logs indicating internal operations of the device main body,
The operation log contains information indicating an operation instruction issued by the information processing apparatus based on analysis conditions and/or operation conditions, and information indicating operation details executed by the apparatus main body in response to the operation instruction. are associated one-to-one,
The operation log further includes at least one of information indicating the purpose of the operation of the device main body and information indicating the result derived by the information processing device based on the operation of the device main body,
The analysis system according to claim 1, wherein the analysis unit analyzes the abnormality of the analysis device based on the operation log when the abnormality of the analysis device is detected. an analyzer;
a diagnostic unit for diagnosing an abnormality sign of the analyzer,
The analysis device is
a device body for analyzing a sample;
an information processing device that controls the operation of the device main body,
The information processing device is configured to collect operation logs indicating internal operations of the device main body,
The operation log contains information indicating an operation instruction issued by the information processing apparatus based on analysis conditions and/or operation conditions, and information indicating operation details executed by the apparatus main body in response to the operation instruction. are associated one-to-one,
The operation log further includes at least one of information indicating the purpose of the operation of the device main body and information indicating the result derived by the information processing device based on the operation of the device main body,
The analysis system, wherein the diagnosis unit diagnoses whether or not there is a sign of abnormality in the analysis device based on the operation log. an analyzer;
A server connected for communication with the analysis device,
The analysis device is
a device body for analyzing a sample;
an information processing device that controls the operation of the device main body,
The information processing device is configured to collect operation logs indicating internal operations of the device main body,
The operation log contains information indicating an operation instruction issued by the information processing apparatus based on analysis conditions and/or operation conditions, and information indicating operation details executed by the apparatus main body in response to the operation instruction. are associated one-to-one,
The analysis device is configured to periodically transmit the collected operation log to the server;
The server has a storage unit for saving the operation log,
An analysis system in which calibration for ensuring analysis accuracy of the analysis device is performed using the operation log saved in the storage unit.

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