JP7620678B2 - Chromatography Equipment - Google Patents

Description

The present invention relates to chromatographic devices such as liquid chromatographic devices and gas chromatographic devices.

Conventionally, in liquid chromatography (HPLC) analysis, an operator refers to an analytical procedure manual that specifies the analytical procedures and conditions (SOP: Standard Operating Procedure) and performs the analysis in accordance with the manual.
On the other hand, an actual liquid chromatograph device operates based on a condition file set in a computer within the device, and during this operation, an operator inputs specific numerical values and conditions from the analysis procedure manual or changes the procedure specified in the device.
Since manually entering such conditions is time-consuming and prone to input errors, technology has been developed that enables analysis conditions to be automatically read from natural language, such as a text file created by the person requesting the analysis, and then set (Patent Document 1).

Patent No. 4660159

However, since the analysis procedure manual and the equipment condition file are managed in separate systems, it is difficult to verify whether the information matches. In addition, when updating the equipment, the condition file must be updated or newly created even if the analysis content is the same. Furthermore, even if the equipment condition file is updated, the operator must reflect this in the procedure manual, which makes it easy for updates to be missed. The same is true in the opposite case.
On the other hand, in a system in which analytical conditions specified in an analytical procedure manual or the like are read and those conditions are stored in the device and then operated, even if the analytical procedure manual is subsequently changed, if the operator is unaware of the change, there is a risk that the analytical conditions previously stored in the device will be used for the next analysis.

The present invention has been made to solve the above problems, and aims to provide a chromatographic device that allows changes to the analysis procedures and conditions of the chromatographic device to be reliably performed on the device side, making analysis easy and error-free.

In order to achieve the above-mentioned object, the chromatographic apparatus of the present invention is a chromatographic apparatus that performs chromatographic analysis in accordance with specified procedures and conditions, and is equipped with a reading unit that reads characters including numerical values and /or units in specified frames from the analytical procedure manual, which is a paper document in which the procedures and conditions are written in the specified frames, at a specified timing when the chromatographic analysis is started in accordance with the analytical procedure manual including the procedures and conditions , and a control unit that performs the chromatographic analysis based on the numerical values and/or the characters read by the reading unit.

With this chromatographic device, analysis can only be performed after reading the analysis procedure manual, which describes the analysis procedures and conditions, so if the analysis procedure manual is changed, the analysis can be performed according to the changes. Also, there is no need for the operator to input the analysis procedures and conditions. This ensures that changes to the analysis procedures and conditions are executed on the device side, allowing the chromatographic device to perform analysis easily and without errors.
Furthermore, since the analytical procedure manual cannot be rewritten by the chromatograph device, the analytical procedure manual can be prevented from being changed erroneously.
Furthermore, since the analysis procedure manual is in a form including a paper document or text data, it is easy to manage as a document (or document data), and the document can be easily modified or copied.

In addition, with the chromatographic device of the present invention, when it is notified that the analytical procedure manual has been certified, the analytical procedure manual can be examined and confirmed to be genuine.

In the chromatography device of the present invention, the control unit may determine whether or not the chromatographic analysis based on the read numerical value and/or character is executable, and notify the result.
According to this chromatographic device, the equipment can automatically determine whether or not the state of the chromatographic device corresponds to the analysis procedure manual and chromatographic analysis can be performed, so that analysis can be performed more easily and without errors using the chromatographic device.

The chromatographic device of the present invention may further include a memory unit that stores information about equipment capable of performing the chromatographic analysis, separate from the chromatographic device, and when the control unit determines that the chromatographic analysis cannot be performed, it may notify the control unit of the equipment that can perform the analysis based on the memory unit.
According to this chromatographic device, even if chromatographic analysis cannot be performed, a notification is automatically sent regarding the availability of equipment that will enable the analysis to be performed. This allows the operator to follow the notification to maintain the chromatographic device so that chromatographic analysis can be easily performed.
In the chromatographic apparatus of the present invention , the position may be at least one of a predetermined frame, a specific page, a header, and a footer of the analytical procedure manual.

In the chromatographic apparatus of the present invention, when there are multiple analytical procedure manuals, the control unit may perform the chromatographic analysis based on one analytical procedure manual, and then prompt the user as to whether or not to read other analytical procedure manuals, or may read other analytical procedure manuals and perform the chromatographic analysis based on multiple predetermined types of the analytical procedure manuals.
This chromatographic apparatus makes it possible to carry out chromatographic analyses in accordance with a plurality of analytical procedure manuals.

According to the present invention, changes to the analysis procedures and conditions of a chromatographic device can be reliably performed on the device itself, making analysis easy and error-free.

1 is a diagram showing a configuration of a liquid chromatograph apparatus according to an embodiment of the present invention. FIG. 1 is a diagram showing an example of an analysis procedure manual made of paper. This is a continuation of Figure 2. This is a continuation of Figure 3. This is a continuation of Figure 4. FIG. 11 is a diagram showing a process flow of a control unit and a reading unit. FIG. 13 is a diagram showing a header indicating the location of an analysis procedure manual. FIG. 13 is another diagram showing a header indicating the location of the analytical procedure manual. FIG. 13 is a diagram showing a sequence table for performing chromatographic analysis according to a plurality of analytical procedure manuals.

Hereinafter, an embodiment of the present invention will be described with reference to the drawings.
FIG. 1 is a diagram showing the configuration of a liquid chromatograph device 100 according to an embodiment of the present invention.
The liquid chromatograph apparatus 100 comprises a data processing device 7 for controlling the entire system, a mobile phase (a mixed solution of eluent and solvent) 1, a pump 2 for delivering the mobile phase 1, an autosampler 3 for injecting samples, a column 4 for separating components, a column oven 5 for keeping the column 4 at a constant temperature, a detector 6 for detecting the separated components, a display unit 10, and a reading unit 11.

The data processing device 7 is composed of a control unit (CPU) 9 that executes the analysis and analyzes the analysis results, a storage unit (hard disk or the like) 8 that stores the analysis results, and a computer having ROM and RAM (not shown). A display unit (monitor) 10 displays the analysis results.
The reading unit 11 reads numerical values, characters and/or units, which will be described later, from the analysis procedure manual. This analysis procedure manual can be in the form of a paper document 20a, a storage medium 20b such as a CD disk or a USB memory that contains text data, or distribution data 20c that contains text data and is distributed from a network 200.
In the case of the analysis procedure manual 20a consisting of a paper document, the reading unit 11 is a scanner (OCR: Optical Character Recognition), in the case of the analysis procedure manual 20b consisting of a storage medium, the reading unit 11 is a reader, and in the case of the analysis procedure manual 20c consisting of distribution data, the reading unit 11 is a network interface and reader.

The detector 6 has a plurality of elements for detecting the signal strength, and is capable of acquiring the signal strength with respect to time.
A sample is injected from an injector (not shown) of an autosampler 3, passes through a column 5 together with a mobile phase 1 delivered by a pump 2, and is separated into various components in the sample.
The sample separated into its components is detected by a detector 6. A signal from the detector 6 is sent to a data processing device 7 where data processing is performed.
The column 4 is a device generally used as a separation section for separating components of a sample present in the mobile phase 1. Examples of the column 4 include a packed column and a monolith column. Various types of column packing materials can be used for the column 4, such as an adsorption type, a distribution type, and an ion exchange type. The column 4 is desirably placed in a column oven 5 so that the column 4 can be kept at a constant temperature and the sample can be separated with good reproducibility.

2 to 5 show an example of the analysis procedure manual 20a made of paper.
FIG. 2 is the cover of the analysis procedure manual 20a, FIG. 3 is the table of contents (structure) of the analysis procedure manual 20a, and FIGS. 4 and 5 are diagrams showing the specific procedures and conditions under the heading “5. Conditions for setting each device during measurement” in FIG.
As shown in Figure 3, the analysis procedure manual 20a has headings 1 to 10, which describe procedures and conditions, and the analysis is carried out according to these headings. Also, the part that says "The part enclosed in a square is an item written in a specified format" is within the box that corresponds to the "position" of the claims.
Moreover, the "procedure" refers to the operations under headings 1 to 10 in the analytical procedure manual 20a. The "condition" refers to the conditions for carrying out the actual operation, such as "analysis time 7 minutes," specified in each box.

As shown in Figures 4 and 5, the heading "5. Conditions for setting each device during measurement" has four boxes, which are arranged in the order of data acquisition conditions, liquid delivery conditions, column heating section conditions, and sample injection section conditions.
It is possible to recognize that the above four boxes are related to data acquisition conditions, liquid delivery conditions, column heat retention conditions, and sample injection conditions by obtaining the character string (title) in the first line of the box. However, for example, liquid delivery conditions are not limited to "liquid delivery conditions" and several words related to "liquid delivery" are recognized. For example, if any of "liquid delivery", "Pump", and "Flow" are included, it is recognized as a liquid delivery condition. This is because the title related to liquid delivery may differ depending on the analysis procedure manual.

The reading unit 11 then reads, for example, the numerical value "7.0" and the character (unit) "min" in the "Data Acquisition Conditions" box in Fig. 4, and the control unit 9 sets the analysis time to 7 min (7 minutes). Similarly, the control unit 9 reads and sets "10 mM acetate buffer" and "acetonitrile" as solvents A and B in the "Liquid Delivery Conditions" box, respectively.
For example, four items of information are set in advance in the "Data Acquisition Conditions" box in Fig. 4: analysis time, analysis wavelength, data acquisition interval, and data response. Also, it is set that the unit of analysis time is "min".
Therefore, when the reading unit 11 reads "7.0" and the unit "min", it recognizes this number as the "analysis time".
However, since the data acquisition interval and data response are both measured in units of "ms", the first "ms" that appears is the data acquisition interval, and the next "ms" that appears is the data response.
In this manner, the various values of the "data acquisition conditions" in Fig. 4 are read out. The same applies to the maximum pressure and minimum pressure of the "liquid delivery conditions" in Fig. 4.

The information in the box "liquid transfer conditions" in FIG. 4 is read as follows.
First, when "Solvent A" to "Solvent D" in the "Liquid Delivery Conditions" box is read, the system is set to read the character string to the right of the capital letters A to D.
Therefore, the reading unit 11 recognizes "solvent A" as "10 mM acetate buffer" and "solvent B" as "acetonitrile."
In addition, the reading unit 11 reads Time, Flow, and "Solvent B %" from the "Liquid Delivery Timetable", reads the specific time (min) for Time, and recognizes that the operation is to mix "solvent B" acetonitrile at the flow rate of Flow at that time with 10 mM acetate buffer solution as solvent A according to the numerical value in the box and the unit % (for example, 40%) to produce a mixed solvent.

This setting may be written as temporary data in, for example, a RAM (random access memory) of the data processing device 7, or may be written in the storage unit 8.
When data is written to the RAM, the data will not remain when the analysis of the liquid chromatograph 100 is completed and the power is turned off. When data is written to the storage unit 8, the data will remain even when the analysis of the liquid chromatograph 100 is completed and the power is turned off.
However, in either case, in the present invention, when starting chromatographic analysis, at a predetermined timing, the reading unit 11 reads the latest analysis procedure manual and performs analysis based on the read data or items previously associated with the read data.

Furthermore, reading an analytical procedure manual "at a predetermined timing" may refer to any time between the time when "chromatographic analysis is started" according to one analytical procedure manual and the time when the actual chromatographic analysis begins.
On the other hand, the analysis procedure manual is read and the analysis is performed based on the manual, but when the analysis is performed, parameters including the assumed values described below may be set as defaults in advance on the device side, even if they are not described in the procedure manual, separately from the analysis procedure manual. Examples of parameters include the following:
a. Firmware parameters (wait time, number of operations, number of loops, memory location address, conversion constant, conversion factor, etc.)
b. Parameters specified during assembly adjustment and maintenance inspection (equipment-specific constants specified at the time of shipment, photointerrupter position tuning constants, zero and span adjustment values related to detection sensitivity, etc.)
c. Default values for customer-configurable parameters (e.g., pump flow rate adjustments, autosampler air gap volumes, column oven temperature calibration adjustments, detector time constant equivalents, etc.)
d. Parameters that can be reasonably assumed even if they are not described in the analytical procedure manual (specified values related to integral calculations in the data processing device, allowable time for the identification time window, etc.)

As a result, the life span during which the analysis conditions are valid is from the start to the end of the chromatographic analysis. In addition, in this embodiment, the measurement data (analysis results) are output to an output device or other data management software at the end of the analysis, and the measurement data is not left in the device 100.

In addition, in this embodiment, the data such as the analysis conditions that have been read can be output together with the analysis results (printed or output as electronic data to a file, etc.), making it possible to know the analysis conditions at that time when viewing the analysis results later.

In the analysis procedure manual 20a, the items to be read are the numbers and/or characters in the boxes, or items that are previously associated with the read numbers and/or characters, which are documents or text data. In contrast, information that is coded and embedded in the document (data) and cannot be identified without using other software, or other documents or link destinations linked from the document, are not read.

Next, the process flow of the control unit 9 and the reading unit 11 will be described with reference to FIG.
First, the reading unit 11 reads the numbers and/or characters within the boxes in the analysis procedure manual 20a as described above (step S2).
Next, the control unit 9 judges whether the reading in step S2 is completed (step S4). This judgment can be made by reading the terminal symbol of the read analytical procedure manual 20a, since the terminal symbol is usually written in an electronic file.
In this embodiment, all information in the analysis procedure manual 20a is read and then the necessary values, etc. are obtained from it, but it is also possible to read one line at a time from the analysis procedure manual 20a, in which case reading the last line indicates that the file system interface function is at the end of the file.
If the answer is "Yes" in step S4, the process proceeds to step S6, and if the answer is "No", the process returns to step S2.

In step S6, the control unit 9 judges whether or not a chromatographic analysis based on the data read in step S2 is executable. This judgment can be made, for example, by storing in advance in the storage unit 8 the equipment (e.g., the type of column 4) corresponding to the items required for the analysis (e.g., headings 1 to 10 in the table of contents in FIG. 3) and by making it possible to recognize the type of equipment (column, etc.) actually installed in the current apparatus 100. Then, the equipment in the data read in step S2 can be compared to see whether it corresponds to the actual equipment.
The type of equipment (column, etc.) actually installed can be recognized, for example, by providing a mechanical protrusion on the column and pressing a corresponding switch on the equipment when the column is attached, or by the operator inputting the column type into the data processing device 7.
If the answer is "Yes" in step S6, the process proceeds to step S8, and if the answer is "No", the process proceeds to step S20.

For example, the available time of a column can be recognized by storing the column type and registration number in advance and specifying the type and registration number during analysis. Also, if an information tag is attached to the column and the column is placed in the column oven, the column information can be automatically read out.

In step S8, the control unit 9 obtains authenticated information from the data read in step S2, and displays (notifies) whether or not the authentication has been performed. For example, when the authenticated information has been obtained, the control unit 9 displays "Authenticated" in a watermark, header, footer, or the like, and when the authenticated information has not been obtained, the control unit 9 displays "Trial".
Similarly, the trial can be displayed as a watermark in the background of the chromatographic display screen, or displayed or highlighted in a specific position.
As a method for obtaining authenticated information, for example, the change history of the document data of the analysis procedure manual can be read out, and if the last change in the change history indicates "authenticated," it can be treated as authenticated. If the document is subsequently changed and the change history is automatically recorded, the last change is updated and no longer indicates "authenticated."

Following step S8, the control unit 9 executes a chromatographic analysis based on the data read in step S2 (step S10).
Next, the control unit 9 judges whether the analysis is completed (step S12). This judgment can be made, for example, by the operator inputting to the data processing device 7 the fact that the analysis according to the analytical procedure manual 20a is to be completed.
If the answer is "No" in step S12, the process returns to step S2; if the answer is "Yes", the process proceeds to step S14. In step S14, the control unit 9 determines whether there is a next analysis that uses a different analysis procedure manual. This determination can be made, for example, by the control unit 9 displaying an "Inquiry about next analysis" screen on the display unit 10, and the operator inputting whether there is a next analysis to be performed into the data processing device 7. If the answer is "Yes" in step S14, the process returns to step S2; if the answer is "No", the process ends.
Then, by returning to step S2, another analytical procedure manual is read and another analysis is started with new procedures and conditions.

On the other hand, if the answer is "No" in step S6, then in step S20 the control unit 9 displays (notifies) the equipment that can perform chromatographic analysis according to the analytical procedure manual 20a.
Specifically, for example, the equipment (e.g., type of column 4) corresponding to the items required for the analysis stored in the memory unit 8 as described above can be read out and displayed as the items required for the analysis (e.g., headings 1 to 10 in the table of contents in FIG. 3).
Following step S20, the control unit 9 determines whether the equipment displayed in step S20 has been installed (step S22). This determination can be made, for example, by acquiring the type of the equipment (column) displayed in step S20.
If the answer is "Yes" in step S22, the process proceeds to step S8, and if the answer is "No", the process ends.

As described above, since an analysis can be performed only after reading the analytical procedure manual that describes the analytical procedures and conditions, if the analytical procedure manual is changed, the analysis can be performed according to the changes. Also, there is no need for the operator to input the analytical procedures and conditions. This ensures that changes to the analytical procedures and conditions are executed on the device side, allowing analysis to be performed easily and without errors using the chromatograph device.
Furthermore, since the analytical procedure manual cannot be rewritten by the chromatograph device, the analytical procedure manual can be prevented from being changed erroneously.
Furthermore, since the analysis procedure manual is in a form including a paper document or text data, it is easy to manage as a document (or document data), and the document can be easily modified or copied.

When it is notified that the analytical procedure manual has been certified, the analytical procedure manual is examined and it can be confirmed that it is genuine.
Also, it may be possible to copy the certified analytical procedure manual.

It goes without saying that the present invention is not limited to the above-described embodiment, but covers various modifications and equivalents within the spirit and scope of the present invention.
The notification method may be a display on the display unit 10 or a voice notification.

The analysis procedure manual is not limited to a paper document, but may be an electronic file such as text data.
The reading position of the analysis procedure manual is not limited to the above embodiment, and may be within a frame, or at least one of a specific page, a specific character string, a header, and a footer.
For example, as shown in Fig. 7, the header of a page that is not intended to be read and is written for general explanation has a header called "Information part." On the other hand, as shown in Fig. 8, the header of a page that is intended to be read for analysis conditions, etc. has a header called "Method part."
Therefore, based on the headers of each page of the analysis procedure manual, by reading the numbers and letters on the page where the header "Method part" is written, it is possible to determine whether the words in the document are written on a page for general explanation or a page for specifying conditions, and obtain the necessary information.

When the analytical procedure manual contains text data, the information described in the header and/or footer can be read.
If the analysis procedure manual is a paper document, the positional relationship of the header and/or footer on one page may be determined in advance, and the information on that position may be read. Furthermore, the position of the page number may also be set in advance, and the header and/or footer may be read in accordance with the page number.
Also, a predetermined distance from the top/bottom side of the paper may be determined in advance as the header/footer, and information on this position may be read.

As an example of the location of the analysis procedure manual, in addition to the specific character strings that are predetermined, headings 1 to 10 in Figure 3 are also examples. In this case, all headings 1 to 10 in Figure 3 are read, and the text from heading "5. Conditions for setting each device during measurement" onwards and before the next heading "6. Peak detection analysis conditions for acquired data" can be read as the contents of heading 5.

The characters to be read may include units. In this case, for example, if the characters "wavelength" and "nm" are written, these can be regarded as the same condition item "wavelength" and the unit can be set to a predetermined one (for example, nm). Also, if "μL/min" is written as the character (unit), this can be unified to "mL/min" and the numerical value can be converted. These examples correspond to "items that are previously associated with the read numerical value and/or characters".

Furthermore, when there are multiple analytical procedure manuals, separate chromatographic analyses can be performed according to each of the multiple analytical procedure manuals by making the judgment in step S14 of Fig. 6. In this case, in step S14, the control unit prompts the user as to whether or not to read another analytical procedure manual, and it is up to the user to decide whether or not to read another analytical procedure manual.
In response to this, a plurality of types of analytical procedure manuals (e.g., the number or names of analytical procedure manuals) may be set in advance on the side of the device 100, and based on this, another analytical procedure manual may be automatically read and a chromatographic analysis may be performed. For this setting, for example, a sequence table as shown in Fig. 9 may be stored in the storage unit 8, and this sequence table may be read out.

In the example of FIG. 9, after the start of chromatographic analysis (start-up of the analysis device), predetermined preparation operations are carried out, and then analysis is performed according to a plurality of analysis procedure manuals in accordance with steps 1 to 5 of the sequence table.
The warm-up operation includes starting pumping, waiting for the temperature of the column oven to stabilize, and waiting for the brightness of the detector lamp to stabilize.
At each step of the sequence table, a vial number is specified separately from the analysis procedure, and the sample from the specified vial number is aspirated, the analysis procedure for that step (analysis procedure "A" at step S1) is read, and the sample is injected under those conditions to perform the measurement. At each step of the sequence table, the number of injections is also specified.

When step 1 is completed, the control unit 9 reads out the vial number and the number of injections for the next step 2, and further reads out the type (name) (A) of the analytical procedure manual. The control unit 9 determines whether the analytical procedure manual A is the same type as the analytical procedure manual A read in the sequence table after the start of the analysis, and since the determination is "Yes," the analytical procedure manual A is not read again in step 2, and the information on the analytical procedure manual A read in step 1 is used.
When step 2 is completed, the control unit 9 reads out the vial number and the number of injections for the next step 3, and further reads out the type (name) (B) of the analytical procedure manual. Since analytical procedure manual B has not yet been read, analytical procedure manual B is read. In this manner, steps up to step 5 are carried out.

It is possible to read all analytical procedure manuals A through C at once from the sequence table before performing step 1, but reading the analytical procedure manuals individually for each step has the following advantages: you can be sure that each analytical procedure manual A through C is always the most recent procedure manual; you can read an analytical procedure manual before going to the next step and change the analysis order; and if another measurement becomes urgently required during a specified measurement, you can read another procedure manual (A through C) and change the measurement order.

The type of analytical procedure manual may be the name (A to C) as described above, or it may be the number of analytical procedure manuals for performing chromatographic analysis (three, A to C, in the example of Figure 9).

9 Control unit 10 Memory unit 11 Reading unit 20a to 20c Analysis procedure manual 100 Chromatograph device

Claims (5)

A chromatographic apparatus for performing a chromatographic analysis according to a predetermined procedure and conditions,
a reading unit that, when starting the chromatographic analysis according to an analytical procedure manual including the procedures and conditions, reads characters including numerical values and/or units included in the positions from the analytical procedure manual, which is a paper document in which the procedures and conditions are written in the positions, at a predetermined timing;
A control unit that performs the chromatographic analysis based on the numerical values and/or the characters read by the reading unit. The chromatographic device according to claim 1, wherein the control unit determines whether the chromatographic analysis based on the read numerical values and/or characters is executable and notifies the result. A storage unit that stores information on equipment capable of performing the chromatographic analysis, separate from the chromatographic device,
The chromatographic apparatus according to claim 2 , wherein when the control unit determines that the chromatographic analysis is not executable, the control unit notifies the equipment that is executable based on the storage unit. 4. The chromatographic apparatus according to claim 1 , wherein the position is at least one of a predetermined frame, a specific page, a header, and a footer of the analytical procedure manual . In the case where there are multiple analytical procedures,
The chromatographic device according to any one of claims 1 to 4, wherein the control unit, after performing the chromatographic analysis based on one analytical procedure manual, prompts the user as to whether or not to read another analytical procedure manual, or reads another analytical procedure manual and performs the chromatographic analysis based on a plurality of types of the analytical procedure manuals that have been preset.

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