CN110873773B - Chromatographic apparatus - Google Patents

Abstract

The invention provides a chromatographic apparatus, which can reliably execute analysis steps and condition change of the chromatographic apparatus at the apparatus side, and can simply and erroneously perform analysis. The chromatographic apparatus (100) performs chromatographic analysis according to prescribed steps and conditions, and comprises: a reading unit (11), when starting chromatographic analysis according to one analysis step book, the reading unit (11) reads the numerical value and/or character of the position from a paper file or an analysis step book (20 a-20 c) containing text data, which records the steps and conditions at the prescribed positions, at the prescribed timing; and a control unit (9) that performs a chromatographic analysis based on the numerical value and/or character read by the reading unit or a matter associated with the numerical value and/or character read in advance.

Description

Chromatographic apparatus

Technical Field

The present invention relates to a chromatographic apparatus such as a liquid chromatography apparatus and a gas chromatography apparatus.

Background

Conventionally, in liquid chromatography (HPLC) analysis, an operator refers to an analysis procedure book defining the procedure and conditions of analysis (SOP: standard operation program), and performs analysis based on the analysis procedure book.

On the other hand, an actual liquid chromatograph device operates based on a condition file set in a computer in the device, and an operator inputs a specific numerical value or a condition of an analysis step book during the operation or changes a step designated in the device.

When such conditions are manually input, a technique has been developed in which analysis conditions can be automatically read from a natural sentence such as a text file created by an analysis requester and the conditions are set, because it may take time or be accompanied by an input error (patent document 1).

Patent document 1: japanese patent No. 4660159

In addition, since the analysis step book and the condition file on the apparatus side are managed by different systems, it is difficult to verify whether or not the information of each other is consistent. In addition, when the device is updated, even if the analysis content is the same, the condition file is forcedly updated and newly created. In addition, even if the condition file on the device side is updated, the operator must perform an operation of reflecting the condition file on the step book side, and update omission is likely to occur. The same is true in the opposite case.

On the other hand, in the case where the analysis conditions defined by the analysis step book or the like are read and stored in the device to operate, even if the analysis step book is changed later, if the operator does not know the change, the analysis conditions stored in the device before the next analysis may be directly used to perform the analysis.

Disclosure of Invention

Accordingly, the present invention has been made to solve the above problems, and an object of the present invention is to provide a chromatographic apparatus including: the steps and conditions of analysis of the chromatographic apparatus can be reliably changed on the apparatus side, and the analysis can be performed simply and without errors.

In order to achieve the above object, a chromatography apparatus according to the present invention performs a chromatography analysis according to a predetermined procedure and condition, wherein the chromatography apparatus comprises: a reading unit that reads, when the chromatographic analysis is started according to an analysis step book including the steps and conditions, numerical values, characters, and/or units in a predetermined frame from a paper file in which the steps and conditions are recorded in the frame or the analysis step book including text data at a predetermined timing; and a control unit that performs the chromatographic analysis based on the numerical value, character, and/or unit read by the reading unit.

According to this chromatograph apparatus, since analysis can be performed only by reading an analysis step book describing the steps and conditions of analysis, analysis according to the contents of the change can be performed when the analysis step book is changed. In addition, the operator is not required to input the steps and conditions of analysis. This makes it possible to reliably perform the steps and the conditions of the analysis on the device side, and to perform the analysis of the chromatographic device easily and without any error.

In addition, since the analysis procedure book cannot be rewritten by the chromatographic apparatus, the analysis procedure book can be prevented from being erroneously changed.

Further, since the analysis step book uses a paper file or a system including text data, it is easy to manage the analysis step book as a document (or document data), and it is easy to change and copy the document.

In the chromatographic apparatus according to the present invention, the analysis procedure book may include authenticated information, and the control unit may be configured to determine whether or not the analysis procedure book is authenticated.

According to this chromatograph apparatus, when the analysis step book is notified that it has been authenticated, the analysis step book is checked in detail, and a proper analysis step book can be identified.

In the chromatographic apparatus according to the present invention, the control unit may determine whether or not the chromatographic analysis can be performed based on the read numerical value, character, and/or unit, and report the result.

According to this chromatograph apparatus, it is possible to automatically determine whether or not the device can perform the chromatographic analysis in accordance with the analysis procedure book with respect to the state of the chromatograph apparatus, and therefore, the analysis of the chromatograph apparatus can be performed more simply and without any error.

The chromatograph according to the present invention is the chromatograph according to claim 3, further comprising a storage unit that stores device information for executing the chromatographic analysis, wherein the control unit notifies the device that can be executed based on the storage unit when it is determined that the chromatographic analysis cannot be executed.

According to this chromatograph apparatus, even if the chromatograph analysis cannot be performed, the executable equipment is automatically notified, and therefore the operator can equip the chromatograph apparatus according to the notification content, and can easily perform the chromatograph analysis.

In the chromatographic apparatus according to the present invention, when there are a plurality of the analysis step books, the control unit may prompt the user to read another analysis step book after performing the chromatographic analysis based on one analysis step book, or may perform reading of another analysis step book and execution of the chromatographic analysis based on a predetermined type of the plurality of analysis step books.

According to this chromatographic apparatus, chromatographic analysis based on a plurality of analysis step books can be performed.

According to the present invention, the steps and conditions for analyzing the chromatographic apparatus can be reliably changed on the apparatus side, and the analysis can be performed simply and without any error.

Drawings

Fig. 1 is a diagram showing a configuration of a liquid chromatograph according to an embodiment of the present invention.

Fig. 2 is a diagram showing an example of an analysis procedure book composed of paper documents.

Fig. 3 is a view next to fig. 2.

Fig. 4 is a view next to fig. 3.

Fig. 5 is a view next to fig. 4.

Fig. 6 is a diagram showing a flow of processing of the control section and the reading section.

Fig. 7 is a diagram showing a header indicating the position of the analysis step book.

Fig. 8 is another diagram showing a title indicating the position of the analysis step book.

Fig. 9 is a diagram showing a sequence table when performing chromatography according to a plurality of analysis step books.

Description of the reference numerals

9: A control unit; 10: a display unit; 11: a reading section; 20a to 20c: analyzing a step book; 100: chromatographic apparatus

Detailed Description

Hereinafter, embodiments of the present invention will be described with reference to the drawings.

Fig. 1 is a diagram showing a configuration of a liquid chromatograph 100 according to an embodiment of the present invention.

The liquid chromatograph 100 includes a data processing device 7 for controlling the whole, a mobile phase (a mixed solution of an eluent and a solvent) 1, a pump 2 for transporting the mobile phase 1, an autosampler 3 for injecting a sample, 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 constituted by a computer having a control unit (CPU) 9 for performing analysis and analyzing the analysis result, a storage unit (hard disk or the like) 8 for storing the analysis result or the analysis result, and a ROM and a RAM, not shown. The display unit (monitor) 10 displays the analysis result or analysis result.

The reading unit 11 reads a numerical value, a character, and/or a unit described later from the analysis procedure book. The analysis step book may be in the form of a paper file 20a, a storage medium 20b such as a CD disk or USB memory containing text data, and distribution data 20c containing text data to be distributed from the network 200.

In the case of the analysis step book 20a composed of paper documents, the reading unit 11 is a scanner (OCR: optical Character Recognition), in the case of the analysis step book 20b composed of a storage medium, the reading unit 11 is a reader, and in the case of the analysis step book 20c composed of distribution data, the reading unit 11 is a network interface and a reader.

The detector 6 has a plurality of elements for detecting signal intensity, and is a detector capable of acquiring signal intensity with respect to time.

The sample is injected from an injector (not shown) of the autosampler 3, and is separated into various components in the sample by passing through a column 4 together with the mobile phase 1 fed from the pump 2.

The sample from which the components have been separated is detected by a detector 6. The signal of the detector 6 is sent to a data processing device 7 for data processing.

The column 4 is a device that is generally used as a separation section for separating components of a sample present in the mobile phase 1. The column 4 may be a packed column, a monolithic column, or the like. As column packing for column 4, various types of packing such as adsorption type, partition type, ion exchange type, and the like can be used. The column 4 is preferably provided in the column oven 5 so that the column 4 is kept at a constant temperature, and thus separation of the sample can be performed with good reproducibility.

Fig. 2 to 5 show an example of an analysis procedure book 20a composed of paper documents.

Fig. 2 is a cover of the analysis step book 20a, fig. 3 is a catalog (structure) of the analysis step book 20a, and fig. 4 and 5 are diagrams showing specific steps and conditions of the title "5" of fig. 3, conditions set in each device section at the time of measurement.

As shown in fig. 3, the procedure and the condition are described in the titles of 1 to 10 of the analysis procedure book 20a, respectively, and the analysis is performed accordingly. The portion surrounded by ≡is an item described in a predetermined format. The "portion" is within a frame corresponding to "position" in the claims.

The "step" refers to an operation of analyzing the titles of 1 to 10 of the step book 20 a. The term "condition" refers to a condition defined in each frame, for example, "analysis time 7min (7 minutes)" or the like, at the time of actual operation.

As shown in fig. 4 and 5, the heading "5" is a condition set in each device section at the time of measurement, and there are 4 frames, which are a data acquisition condition, an infusion condition, a column heat-retaining section condition, and a sample injection section condition in this order.

The 4 frames are related to the data acquisition conditions, the infusion conditions, the column incubation portion conditions, and the sample injection portion conditions, respectively, and the character string (header) of the first line in the frame can be acquired and recognized. However, for example, if the condition is an infusion condition, the method is not limited to the "infusion condition", and several words related to the "infusion" are recognized. For example, if any one of "infusion", "pump", and "flow rate" is included, the infusion condition is identified. This is because the title related to infusion may vary depending on the analysis procedure book.

Then, the reading unit 11 reads, for example, the numerical value "7.0" and the character (unit) "min" in the frame of the "data acquisition condition" in fig. 4, and the control unit 9 sets the analysis time to 7min (7 minutes). Similarly, the solvents A, B in the frame of "infusion conditions" were read and set as "10mM acetate buffer", "acetonitrile", respectively.

For example, as information in the box of "data acquisition conditions" in fig. 4, 4 pieces of analysis time, analysis wavelength, data acquisition interval, and data response are set in advance. The unit of analysis time is also set to "min".

Therefore, when the reading section 11 reads "7.0" and the unit "min", it is recognized that the value is "analysis time".

However, since the data acquisition interval and the unit of the data response are both "ms", it is also set that "ms" appearing first is the data acquisition interval and "ms" appearing next is the data response.

Thus, each numerical value of the "data acquisition condition" of fig. 4 is read. The same is true for the maximum and minimum pressures of the "infusion conditions" of fig. 4.

In addition, the information in the frame of "infusion condition" of fig. 4 is read as follows.

First, when reading "solvent a" to "solvent D" in the frame of "infusion condition", the character string on the right of the capital letters a to D of the alphabet is set to be read.

Therefore, the reader 11 recognizes "solvent a" as "10mM acetate buffer", and "solvent B" as "acetonitrile".

The reading unit 11 reads the time and flow rate of the "infusion schedule", and the specific time (min) of the time, and recognizes the following operation: during this time, acetonitrile as "solvent B" was mixed with 10mM acetic acid buffer of solvent a according to the flow rate of the liquid stream according to the numerical value and unit (e.g., 40%) in the frame to form a mixed solvent.

The setting may be written as temporary data in a RAM (random access memory) of the data processing apparatus 7, or may be written in the storage unit 8.

In the case of writing into the RAM, when the power supply is turned off after the analysis of the liquid chromatography apparatus 100 is completed, no data is retained. In the case of writing into the storage unit 8, data is retained even if the power supply is turned off after the analysis of the liquid chromatography device 100 is completed.

In any case, however, in the present invention, at the start of the chromatographic analysis, the reading unit 11 reads the latest analysis procedure book at a predetermined timing, and performs the analysis based on the read data or the items associated with the read data in advance.

The reading of the analysis step book at the "predetermined timing" means any time from the time when the "start of the chromatography" according to the 1 analysis step book is started to the time when the actual chromatography is started.

On the other hand, when the analysis step book is read and analyzed, parameters including virtual values described later may be set on the device side in a predetermined manner, unlike the analysis step book, even if the analysis step book is not described. For example, the following parameters are mentioned.

A. Parameters of the firmware (latency, number of operations, number of cycles, address of storage location, conversion constant, conversion coefficient, etc.)

B. Parameters specified during assembly adjustment and maintenance inspection (constants inherent to a device specified at shipment, position tuning constants of a light shielding blade, zero-shift adjustment values related to detection sensitivity, etc.)

C. Default values for parameters settable by the customer (flow adjustment value for pump, air gap volume for autoinjector, adjustment value for temperature correction for column oven, time constant for detector, etc.)

D. parameters which are normally conceivable even though they are not described in the analysis step book (specified value associated with the integral calculation of the data processing apparatus, allowable time of the authentication time window, etc.)

Thus, the useful lifetime of the analysis conditions is from the beginning to the end of the chromatographic analysis. In the present embodiment, measurement data (analysis result) is output to the output device or other data management software at the end of analysis, and the measurement data is not left in the device 100.

In the present embodiment, the data such as the read analysis conditions may be output together with the analysis result (printed or output as electronic data in a file or the like), and then the analysis conditions at that time may be known when the analysis result is seen.

Further, the analysis step book 20a is subject to reading of numerical values and/or characters in a frame or matters associated with the numerical values and/or characters read in advance, and these are documents or text data. On the other hand, by encoding the document (data), it is necessary to use information that can be discriminated by other software, other documents linked from the document, a link destination, and the like are not read targets.

Next, the processing flows of the control unit 9 and the reading unit 11 will be described with reference to fig. 6.

First, the reading unit 11 reads the numerical value and/or the character in the frame of the analysis step book 20a as described above (step S2).

Next, the control unit 9 determines whether or not the reading in step S2 is completed (step S4). Since the end mark of the read analysis step book 20a is usually described in an electronic file, the end mark can be read to make this determination.

In the present embodiment, all the information of the analysis step book 20a is read, and then a desired value or the like is obtained therefrom, but it is also possible to read from the analysis step book 20a line by line, in which case the interface function indicating the file system is the end of the file when the last line is read.

In step S4, if yes, the process proceeds to step S6, and if no, the process returns to step S2.

In step S6, the control unit 9 determines whether or not the chromatographic analysis can be performed based on the data read in step S2. As for this determination, for example, the types of devices (for example, the types of the columns 4) corresponding to the items (for example, the titles 1 to 10 of the catalog of fig. 3) required for analysis are stored in the storage unit 8 in advance, and the types of the devices (columns and the like) actually mounted on the current apparatus 100 can be identified in advance. Then, this determination can be made by comparing whether the device in the data read in step S2 corresponds to an actual device.

As a method for identifying the type of the device (column, etc.) to be actually mounted, for example, a mechanical protrusion may be provided on the column, a corresponding device-side switch may be pressed when the column is mounted, or the operator may input the type of the column to the data processing device 7.

In step S6, if yes, the process proceeds to step S8, and if no, the process proceeds to step S20.

For example, regarding the usable time of the column, the column type or registration number may be stored in advance, and the column type or registration number may be designated for identification at the time of analysis. In addition, when an information tag is attached to the column and is provided in the column oven, the information of the column can be automatically read.

In step S8, the control unit 9 acquires the authenticated information from the data read in step S2, and displays (reports) the presence or absence of authentication. In the method of display, for example, when authenticated information can be acquired and when "authenticated" cannot be acquired, the display of "Trial" is displayed by a watermark, header, footer, or the like.

Similarly, trial can be displayed as a watermark on the background of the display screen of the chromatograph, or can be displayed and emphasized at a specific position.

As a method of acquiring authenticated information, for example, if the change history of the document data of the analysis step book is read out and the final change of the change history is expressed as "authentication", it can be regarded as authenticated. Thereafter, in the case where the change history is automatically recorded when the document is changed, the final change is updated instead of being "authenticated".

Next to step S8, the control unit 9 performs chromatographic analysis based on the data read in step S2 (step S10).

Next, the control unit 9 determines whether or not the analysis is completed (step S12). This determination can be performed, for example, by the operator inputting the meaning of ending the analysis of the analysis step book 20a to the data processing device 7.

In step S12, if no, the process returns to step S2, and if yes, the process proceeds to step S14. In step S14, the control unit 9 determines whether or not there is a next analysis using the other analysis step book. This determination can be performed, for example, by the control unit 9 displaying a screen of "whether or not there is a query for the next analysis" on the display unit 10 and the operator inputting whether or not there is a query for the next analysis into the data processing device 7. In step S14, if yes, the process returns to step S2, and if no, the process ends.

Then, when returning to step S2, the other analysis step book is read, and other analysis is started according to the new steps and conditions.

On the other hand, in the case of no in step S6, in step S20, the control section 9 displays (reports) a device capable of performing chromatographic analysis based on the analysis step book 20 a.

Specifically, for example, the following can be performed: the necessary equipment (for example, the type of the column 4) is read out, and the equipment (for example, the type of the column 4) corresponding to the analysis necessary item stored in the storage unit 8 as described above is displayed as the analysis necessary item (for example, the titles of 1 to 10 of the catalog of fig. 3).

Next to step S20, the control unit 9 determines whether or not the device displayed in step S20 is mounted (step S22). This determination can be performed by, for example, acquiring the type of the device (column) displayed in step S20.

In step S22, if yes, the process proceeds to step S8, and if no, the process ends.

As described above, since the analysis can be performed only by reading the analysis step book in which the steps and conditions of the analysis are described, when the analysis step book is changed, the analysis according to the change contents can be performed. In addition, the operator is not required to input the steps and conditions of analysis. This makes it possible to reliably perform the steps and the conditions of the analysis on the device side, and to perform the analysis of the chromatographic device easily and without any error.

In addition, since the analysis procedure book cannot be rewritten by the chromatograph, the analysis procedure book can be prevented from being erroneously changed.

Further, since the analysis step book uses a paper file or a system including text data, it is easy to manage the analysis step book as a document (or document data), and it is easy to change or copy the document.

When the analysis step book is notified that the authentication is completed, the analysis step book is checked in detail, and the normal analysis step book can be identified.

In addition, the authenticated analysis step book may be reproducible.

The present invention is not limited to the above-described embodiments, but, of course, relates to various modifications and equivalents included in the spirit and scope of the present invention.

The method of notification includes, in addition to the display on the display unit 10, notification by sound.

The analysis step book is not limited to a paper file, but may be an electronic file such as text data.

The reading position of the analysis step book is not limited to the above embodiment, but may be at least 1 of a specific page, a specific character string, a header, and a footer, other than the inside of the frame.

For example, as shown in fig. 7, a header of a page described for general description, not a read target, is described with an "information portion". On the other hand, as shown in fig. 8, a header of a page to be read such as an analysis condition is described with a header of a "method portion".

Therefore, by reading the number and character of the page in which the header of each page of the step book is described, and by determining whether the language in the document is a page described for general description or a page for specifying the condition, the required information can be acquired.

In the case where the analysis step book contains text data, the information described in the header and/or footer may be read.

In the case where the analysis step book is a paper document, it is sufficient to determine in advance the positional relationship of the header and/or footer in 1 page and read the information of the position. In addition, the position of the page number may be set in advance, and the header and/or footer may be read in correspondence with the page number.

In addition, a predetermined distance from the upper edge, lower edge, or the like of the paper may be determined as a header/footer in advance, so that information on the position may be read.

As an example of the position of the analysis step book, there are, for example, titles 1 to 10 of fig. 3, as well as predetermined character strings. In this case, all of the titles 1 to 10 in fig. 3 can be read, and the document in the portion before the title "5" is read as the content of the title 5 after the condition "6" set in each device section at the time of measurement and the next title "6" is read.

The read character may also contain units. In this case, for example, when "wavelength" and "nm" are described as characters, they are regarded as the same condition item, "wavelength" (or "wavelength"), and the unit thereof may be set to a predetermined unit (for example, nm). Note that, when "μl/min" is described as a character (unit), the unit is collectively "mL/min", and the numerical value may be converted. These examples correspond to "matters associated with the read numerical value and/or character in advance".

In addition, when there are a plurality of analysis step books, by performing the determination in step S14 of fig. 6, it is possible to perform individual chromatographic analyses based on the plurality of analysis step books. In this case, in step S14, the control unit reminds the user of the presence or absence of reading of another analysis step book, and the user determines whether or not to read another analysis step book.

In contrast, the device 100 may automatically read another analysis step book and execute the chromatographic analysis by setting a plurality of types of analysis step books (for example, the number and the name of the analysis step books) in advance. As this setting, for example, the sequence table shown in fig. 9 is stored in the storage unit 8 in advance, and this sequence table can be read out.

In the example of fig. 9, after the chromatographic analysis (start-up of the analysis device) is started, a predetermined preparatory operation is performed, and then, analysis based on a plurality of analysis step books is performed according to steps 1 to 5 of the sequence table.

Examples of the preparation operation include starting the pumping and the infusion, waiting for the temperature stabilization of the column oven, and waiting for the stabilization of the brightness of the lamp of the detector.

In each step of the sequence table, a vial number is designated, unlike the analysis step book, and the sample of the designated vial number is suctioned, and the analysis step book of the step (analysis step book "a" in step S1) is read, and the sample is injected under this condition to perform measurement. The number of injections is also specified in each step of the sequence table.

When step 1 is completed, the control unit 9 reads the vial number and the number of injections in the next step 2, and further reads the type (name) of the analysis step book (a). The control unit 9 determines whether or not the analysis step book a is of the same type as the analysis step book a read in the sequence table after the start of the analysis, and if yes, the analysis step book a is not read again in step 2, and the information of the analysis step book a read in step 1 is used.

When step 2 is completed, the control unit 9 reads the vial number and the number of injections in the next step 3, and further reads the type (name) of the analysis step book (B). Since the analysis step book B has not been read yet, the analysis step book B is read. This proceeds to step 5.

The type (A, B, C) of the analysis step book can be read out from the sequence table at a time, and all the analysis step books a to C are read out before the step 1 is performed, but when the analysis step books are read out for each step, the following advantages are obtained: the latest analysis step book A-C can be confirmed all the time; if the analysis step book is before entering the next step, the analysis step book can be read to change the analysis sequence; when another measurement is required in a predetermined measurement, the order of measurement can be changed by reading a different procedure from a to C.

The types of analysis procedure books may be a number of analysis procedure books (3 in the example of fig. 9, a to C) for performing chromatography, in addition to the names (a to C).

Claims (6)

1. A chromatographic apparatus for performing chromatographic analysis according to prescribed steps and conditions, wherein,

The chromatographic apparatus has:

a reading unit that reads, when the chromatographic analysis is started according to an analysis step book including the steps and conditions, numeric values and/or characters included in a predetermined position from a paper file or the analysis step book including text data, which records the steps and conditions in the position, at a predetermined timing; and

A control unit that performs the chromatographic analysis based on the numerical value and/or the character read by the reading unit or a matter associated with the numerical value and/or character read in advance,

Information on whether or not it is authenticated is contained in the analysis step book,

The control unit reports whether the analysis step book is authenticated,

If the change history of the document data of the analysis step book is read out and the final change of the change history is represented as "authenticated", it is regarded as authenticated, and thereafter, in the case where the change history is automatically recorded when the document is changed, the final change is updated instead of "authenticated".

2. The chromatographic apparatus according to claim 1, wherein,

The control unit determines whether or not the chromatographic analysis can be performed based on the read numerical value and/or character, and reports the result.

3. The chromatographic apparatus according to claim 2, wherein,

The chromatographic apparatus further has a storage section storing device information for performing the chromatographic analysis,

The control unit notifies the executable device based on the storage unit when it is determined that the chromatographic analysis cannot be executed.

4. A chromatographic apparatus as claimed in any one of claims 1 to 3 wherein,

The character comprises units.

5. A chromatographic apparatus as claimed in any one of claims 1 to 3 wherein,

The position is at least 1 of a specified frame of the analysis step book, a specific page, a specific character string, a header, and a footer.

6. A chromatographic apparatus as claimed in any one of claims 1 to 3 wherein,

In the case where there are a plurality of the analysis step books,

The control unit reminds the user of the presence or absence of reading another analysis step book after the chromatographic analysis is performed based on one analysis step book, or reads another analysis step book and performs the chromatographic analysis based on a predetermined type of a plurality of analysis step books.