JP2011117815A - Liquid chromatograph apparatus, and method of managing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a liquid chromatograph apparatus capable of preventing analysis interruptions by accurately obtaining the remaining quantity of a reagent in a sample container and the amount of space of a waste liquid container, predicting the amount of a reagent used and the amount of occurrence of a waste liquid on the basis of analysis conditions, and issuing an alarm on the shortage of reagents and the overflow of the waste liquid container, and to provide a management method of the liquid chromatograph apparatus. <P>SOLUTION: The liquid chromatograph apparatus is configured: to detect the amount of liquids in the containers by providing a plurality of RFID tags for the reagent container and the waste liquid container; to predict the total amount of reagents used and the amount of occurrence of a waste liquid on the basis of the number of specimens to be analyzed and the amount of regents used for each specimen; to make a display device display a shortage message that a reagent of the reagent container is short; and to make the display device display an overflow message when the waste liquid container will overflow. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

  The present invention relates to a liquid chromatograph device and a management method thereof, and more particularly, to a reagent used in a liquid chromatograph device and a management technique for generated waste liquid.

  The liquid chromatograph apparatus is an apparatus that analyzes a sample to be analyzed by a separation column, detects a separated component, and performs component analysis. In a general-purpose liquid chromatograph device in which the sample to be analyzed is not specified, multiple processes such as a conditioning process including the dilution process, reaction process, and column equilibration of the sample to be analyzed, the analysis process, and the flow path cleaning process are set. The user has to do in detail in advance. In addition, when the sample to be analyzed changes, the user must set the process again in accordance with the change. In particular, it is not a user who has knowledge about chromatograms to judge whether the amount of many kinds of reagents consumed when continuously analyzing many kinds of samples is sufficient for the amount of residual liquid in each reagent container. And difficult.

  On the other hand, when a specific sample such as an amino acid is repeatedly analyzed, it is not necessary to change the analysis conditions, so that the analysis process can be easily automated. As examples of automated liquid chromatographs, amino acid analyzers, glycohemoglobin analyzers and the like are known. However, even in amino acid analyzers that are being automated, the eluent that sends the sample to be analyzed to the separation column, the consumption of the reaction reagent that reacts with the separated components of the sample, the remaining amount, and the container that holds the waste liquid It is difficult to automate the management of reagent containers and waste liquid containers such as empty capacity, and the current situation is that the user visually confirms the containers. Since visual confirmation cannot completely eliminate human error, there is a possibility that the reagent may be insufficient or the waste liquid may overflow during analysis.

  On the other hand, in a liquid chromatograph apparatus, a technique has been proposed in which the weight of a reagent container is measured to determine the amount of the reagent, the consumption is predicted, and a reagent replenishment warning is issued (for example, patent document) 1). In addition, a technique for detecting the presence or absence of liquid in a container using a wireless IC tag such as an RFID (Radio Frequency Identification) tag has been proposed (for example, see Patent Document 2). In the method of measuring the weight of the container to obtain the liquid amount, the specific gravity of the liquid must be taken into account, and the user has to input the specific gravity into the calculation formula every time the reagent changes. Moreover, although the presence or absence of the liquid in a container can be detected by using a wireless IC tag, the amount is not detected and cannot be used for reagent management.

JP 2007-040811 A JP 2006-290402 A

  The present invention accurately grasps the remaining amount of reagent in the reagent container and the empty capacity of the waste liquid container, predicts the amount of reagent used and the amount of waste liquid generated based on the analysis conditions, and runs out of reagents and overflow of the waste liquid container. It is an object of the present invention to provide a liquid chromatograph apparatus and a management method for the liquid chromatograph apparatus that can prevent analysis from being interrupted.

  In order to solve the above problems, a liquid chromatograph apparatus according to the present invention is provided with a plurality of RFID tags in a reagent container or a waste liquid container to detect the amount of liquid in the container, and the number of samples to be analyzed and per sample. The total amount of reagent used and the amount of waste liquid generated are predicted from the amount of reagent used, and if the reagent in the reagent container is insufficient, a message that is insufficient is displayed on the display device. If the waste container overflows, an overflow message is displayed. Is displayed on the display device.

  According to the present invention, the remaining amount of reagent in the reagent container and the empty capacity of the waste liquid container are accurately grasped, the amount of reagent used and the amount of waste liquid generated are predicted based on the analysis conditions, and the reagent shortage and waste liquid container are estimated. By alerting the overflow of the liquid chromatograph, it is possible to provide a liquid chromatograph apparatus and a liquid chromatograph apparatus management method capable of preventing interruption of analysis.

It is a block diagram which shows schematic structure of a liquid chromatograph apparatus. It is a flowchart showing an analysis process. It is a block diagram showing the outline | summary of the system which detects the quantity of the eluent of an eluent container. It is a flowchart which shows the process of the reagent remaining amount management performed in an information analysis part. It is a screen figure which shows an example of the screen displayed on a display. It is a screen figure which shows an example of the screen displayed on a display. It is a screen figure which shows an example of the screen displayed on a display. It is a screen figure which shows the edit screen of a flow program. It is the screen figure which displayed the calculation formula which estimates the consumption of a reagent, and the result. It is a screen figure which shows an example of the screen which displays the value which reduce | subtracted the estimated reagent consumption from the detected present reagent residual amount. FIG. 11 is a message screen diagram that is displayed when an “add / discard liquid” button is instructed in FIG. 10. It is a screen figure which shows an example of a message screen. It is a block diagram showing the outline | summary of the system which detects the liquid quantity of a waste-liquid container. It is a flowchart which shows the waste liquid amount measurement process in an information analysis part. FIG. 11 is a message screen diagram that is displayed when an “add / discard liquid” button is instructed in FIG. 10. It is a screen figure which shows an example of a message screen.

  Embodiments according to the present invention will be described below with reference to the drawings.

  FIG. 1 is a configuration diagram showing a schematic configuration of a liquid chromatograph apparatus. The main parts of the apparatus are an eluent pump 1 for feeding an eluent for transporting the sample to the separation column 11, an autosampler 9 for injecting the sample into the eluent, a separation column 11 for separating the sample into its components, and a chemical component In order to detect by reaction, there are a reaction reagent pump 2 for sending a reaction reagent, a reaction column 13 in which the component chemically reacts with the reaction reagent, a visible detector 14 for detecting the component, and a control unit 15 for controlling the components. .

  Specific examples of the present invention will be described below using an amino acid analyzer as an example. An amino acid analyzer is an apparatus that enables automatic quantitative and qualitative analysis of amino acid compositions contained in biological fluids such as protein hydrolyzate amino acids, serum, and urine.

  The eluent is put in a plurality of eluent containers 3 provided with valves, and the opening and closing of the valves is controlled by a command from the control unit 15 to determine which eluent container 3 is used. The Further, the regenerative liquid container 5 is installed in the same manner as the eluent liquid container 3, only the valve of the regenerative liquid container 5 is opened, the regenerated liquid is fed by the eluent pump 1, and the sample is not injected by the autosampler 9. In this way, the separation column 11 and the piping are cleaned.

  In the case of amino acid analysis, the reaction reagent contains a reaction reagent ninhydrin in a plurality of reaction reagent containers 6 provided with valves, and the control unit 15 controls the opening and closing of the valves to determine which reaction reagent container 6 It is decided whether to use. Moreover, the reaction system washing | cleaning liquid container 7 is installed similarly to the reaction reagent container 6, only the valve | bulb of the reaction system washing | cleaning liquid container 7 is opened, reaction system washing | cleaning liquid is sent with the reaction reagent pump 2, reaction column 13 and piping Perform cleaning. In the case of an amino acid analyzer, distilled water for cleaning the reaction system flow path or 5% ethanol aqueous solution is used as the cleaning liquid.

  In order to perform the separation of the sample components in the separation column 11 at a constant temperature, the separation column 11 is installed in the separation column constant temperature apparatus 10. The reaction column 13 is also installed in the reaction apparatus 12 in order to adjust reaction conditions such as environmental temperature. The column temperature is determined by a time program set in advance according to the analysis content, and is controlled by a command from the control unit 15.

  A nitrogen gas container 4 is connected to the eluent container 3, the regenerative liquid container 5, the reaction reagent container 6, and the reaction system cleaning liquid container 7, and nitrogen gas is pressurized in the connection pipe. When the valve of any container is opened, the eluent and the reagent inside the container are sent to the pump by nitrogen gas, and are sent to the column by the eluent pump 1 and the reaction reagent pump 2. A pressure sensor and a flow rate sensor (not shown) are provided on the discharge side of the eluent pump 1 and the reaction reagent pump 2, and each measured value is sent to the control unit 15.

  When the sample to be analyzed is an amino acid, ammonia contained in the eluent inhibits detection of amino acid components. Therefore, an ammonia filter column 8 is provided immediately after the eluent pump 1 to remove ammonia contained in the eluent.

  A plurality of analysis target samples are set in the autosampler 9 immediately before the separation column 11, and the analysis target samples are automatically injected into the eluent at predetermined time intervals. The sample sent to the separation column 11 together with the eluent is separated and developed into each component by the separation column 11 and eluted with a time difference. Thereafter, it is mixed with the reaction reagent fed by the reaction reagent pump 2 and heated to react with the reaction device 12.

  The amino acid colored by the reaction becomes the color of the dye Luemann purple, and is sequentially sent to the visible detector 14 where it is colorimetrically measured at wavelengths of 570 nm and 440 nm, and the visible absorbance detected by the visible detector 14 is controlled by the controller 15. To be displayed on a display (not shown) or printed to inform the user of the analysis result. The sample component that has passed through the visible detector 14 is discharged to the waste liquid container 16.

  FIG. 2 is a flowchart showing the analysis process. When the user turns on the amino acid analyzer (step 201), the condition setting step (1) is executed, and the sample table is created and registered (step 202). The user uses the input / output device of the control unit 15 to select analysis conditions preset in the storage unit, set the number of samples, and create a sample table that tabulates information for performing continuous analysis. And stored in the storage unit.

  Next, an apparatus confirmation process (2) is performed. First, the remaining amount of the reagent is confirmed. In the conventional apparatus, the user visually checks the reagent container to check the remaining amount of the reagent, but in the present invention, it is automatically checked by the method described later. Then, from the analysis conditions of the sample table registered in the storage unit of the control unit 15 and the number of samples, the processor of the control unit 15 automatically calculates the consumption amount of the reagent and subtracts it from the current remaining amount of the reagent. The predicted reagent remaining amount is calculated, and it is determined whether the predicted reagent remaining amount is less than zero (step 203).

  If the predicted reagent remaining amount is less than zero, or if it is zero, a “reagent remaining amount warning” prompting replenishment of the reagent or replacement of the reagent container is displayed (step 204). When the “reagent remaining amount warning” is displayed, the user replaces the reagent container with a new one or performs an operation of replenishing the reagent.

  Next, the amount of waste liquid in the waste liquid container 16 is confirmed. In the conventional apparatus, the user visually confirms the amount of waste liquid by visually checking the waste liquid container, but in the present invention, it is automatically confirmed by the method described later. The processor of the control unit 15 automatically calculates the predicted waste liquid amount from the calculated reagent consumption amount, adds this to the current waste liquid amount to calculate the predicted waste liquid amount, and compares it with the capacity of the waste liquid container (step 205). ). If this predicted amount of waste liquid is the same as or exceeds the capacity of the waste liquid container, it overflows, so that a “waste liquid amount warning” prompting to discard the waste liquid is displayed (step 206). When the “Waste Liquid Warning” is displayed, the user performs an operation of discarding the waste liquid in the waste liquid container.

  Next, the control unit 15 checks consumable parts (step 207). Specifically, when a part that needs periodic replacement, such as a pump pipe seal, is replaced, the user registers it in the control unit 15, and then the control unit adds the number of specimens, Try to manage frequency of use. Since the user registers the number of samples in step 202 at the start of analysis, the control unit 15 calculates the predicted number of times of use by adding the number of registered samples to the previous use frequency. Since the use limit of the part is set in the storage unit of the control unit 15 in advance, the use limit is compared with the predicted use count, and if it is the same or exceeds, a “replacement part warning” prompting replacement of the part is displayed. . When the “replacement part warning” is displayed, the user replaces the specified part.

  Next, the amino acid analyzer performs a preparation step (3). A bubbling process is performed using the nitrogen gas in the nitrogen gas container 4 (step 208), the regeneration liquid is supplied to the eluent pump 1 to clean the plunger, and the reaction system cleaning liquid is supplied to the reaction reagent pump 2 to clean the plunger. (Step 209), and the autosampler 9 is washed with the regenerating solution (Step 210). Further, a pump purge process is performed as a pre-process for the eluent pump 1 and the reaction reagent pump 2 (step 211), and warming up is performed in which the pump flow rate is gradually increased (step 212). Then, regeneration processing of the separation column 11 and the reaction column 13 is performed (step 231), and the process proceeds to the analysis step (4).

  In the analysis step (4), first, the number of samples that have been analyzed is compared with the number of registered samples registered in the sample table (step 214). If they do not match, the analysis is performed (step 215). Exit.

  When the analysis of all specimens is completed, the cleaning step (5) is executed. In the washing step (5), the separation column 11 and the reaction column 13 are automatically washed (step 216), and the eluent pump 1 and the reaction reagent pump 2 are stopped after a predetermined time (step 217).

  FIG. 3 is a configuration diagram showing an outline of a system for detecting the amount of eluent and the like in the eluent container 3. By newly providing the system shown in FIG. 3 in an amino acid analyzer or a liquid chromatograph apparatus, a “reagent remaining amount warning” and a “waste liquid amount warning” can be performed. As the reagent, there is a reaction reagent in addition to the eluent, but FIG. 3 illustrates the case of the eluent as an example.

  As a sensor for monitoring the amount of reagent in the container 31, an RFID (Radio Frequency Identification) tag, which is a kind of wireless IC tag described in Patent Document 2, is used. In the embodiment of the present invention, not only the presence / absence of the liquid in the container but also the amount of liquid in the container is detected using a plurality of RFIDs. A plurality of RFID tags 30a, 30b,..., 30j are attached at intervals according to the purpose of detecting the reagent amount along the direction in which the liquid level of the outer surface of the container 31 increases or decreases. In the lowermost RFID tag 30j, information that the remaining liquid amount is close to zero is stored in advance.

  A read / write device 32 that reads information by wireless communication with the RFID tag is installed on the opposite side of the container 31 through the reagent. Since the radio wave of the RFID tag uses a 2.45 GHz high frequency band that cannot pass through the liquid, the part with the liquid cannot pass and the part without the liquid can pass. Therefore, for example, when radio waves pass from the RFID tag 30a to the RFID tag 30c but radio waves cannot pass from the RFID tag 30d to the RFID tag 30j, there may be a liquid surface between the RFID tag 30c and the RFID tag 30d. Recognize.

  Information from the RFID tag 30 a to the RFID tag 30 c detected by the read / write device 32 is sent to the communication control unit 33 of the control unit 15, and the amount of reagent in the container 31 is calculated by the information analysis unit 34, and the remaining reagent Used for quantity management. The reagent amount is sent to the calculation unit 35 and stored in the storage unit 39.

  The RFID tag not only returns radio waves when communicating with the read / write device 32 but also has a function of storing the ID of the container 31, the reagent name, and the date and time of communication. Even if the container 31 is stored and removed from the apparatus, the previous use date and time can be read from the RFID tag when it is used next time. Using this function, even if the container is used with another amino acid analyzer, the remaining amino acid analyzer can accurately grasp the amount of residual liquid. It can be done easily. In the example of FIG. 3, the reagent has been described as an example, but the remaining amount of the reaction reagent container 6 and the waste liquid container 16 can be managed by the same system.

  In the example of FIG. 3, the RFID tag 30j is the lowest RFID tag, and when the read / write device 32 detects the RFID tag 30j, the information that the remaining amount of liquid stored in the RFID tag 30j is close to zero is read. It is done. When the information analysis unit 34 receives information from the read / write device 32 via the communication control unit 33 that the remaining amount of liquid is close to zero, the information analysis unit 34 receives information that the remaining amount of liquid is close to zero. Along with the communication date and time, the ID of the container 31, and the reagent name, the information is transmitted to the calculation unit 35 of the control unit 15. The computing unit 35 causes the display 37 to display a message that the remaining amount of the reagent solution in the container 31 is near zero on the display 37 via the input / output unit 36. A user who sees the message that the remaining amount of liquid is close to zero inputs a signal indicating that the confirmation has been made from the input device 38 such as a mouse or keyboard of a personal computer.

  When the read / write device 32 detects the RFID tag 30j at the lowest position of the container 31 shown in FIG. 3, the remaining amount is close to zero, so that no further analysis can be performed. At the time of analysis, as described above, how much reagent is used can be calculated in advance, so which of the plurality of RFID tags 30a, 30b,... 30j attached to the container 31 shown in FIG. By dividing the estimated amount of reagent used from the remaining amount of reagent that can be determined by communicating with the user, it is possible to determine whether preparation of another reagent container is necessary. As described above, by managing the remaining amount of the container 31 by using a plurality of RFID tags attached to the container 31, it is possible to know how much reagent has to be prepared. Can be avoided.

  The waste liquid container 16 shown in FIG. 1 normally has only one container with a large capacity. When an RFID tag is provided in the waste liquid container 16, the amount of waste liquid increases, so that it does not overflow. Need to be monitored. Details will be described later.

  FIG. 4 is a flowchart showing the remaining reagent management process executed by the information analysis unit 34. Radio waves are transmitted to all the RFID tags attached to the container 31 as shown in FIG. 3, and the information stored in each RFID tag is read (step 401). When the container 31 is a reagent container, reading is sequentially performed downward from the uppermost RFID tag 30a of the container 31. Then, for each RFID tag, it is confirmed whether or not there is a reply to the transmission of the radio wave (step 402), and if there is a reagent liquid level between the RFID tag that has responded and the RFID tag that has not responded Judgment is made and the reagent amount is calculated (step 403).

  If reading is stopped with the RFID tag when no reply is received without reading all the RFID tags, the time for reading the RFID tag where the reagent is present can be omitted. However, for example, when there is a reply from the RFID tag 30a to the RFID tag 30c, there is no reply from the RFID tag 30d, and there is a reply from the RFID tag 30e, if the RFID tag 30d stops reading, the RFID tag 30d will fail. If the reply cannot be made, the remaining amount is mistakenly recognized. Therefore, by performing communication with all RFID tags, erroneous recognition due to failure of the RFID tag is prevented.

  FIG. 5 is a screen diagram showing an example of a screen displayed on the display 37, which becomes a start screen for reagent and waste liquid management. The screen 50 displays a reagent and waste liquid management screen, the area 51 displays the analysis result, the area 52 displays the system status of the amino acid analyzer, and the area 53 displays an instruction button. Yes. When the “reagent consumption calculation” button 54 is instructed by the input device 38 such as a mouse or a keyboard, a screen for displaying liquid volume management information is displayed. When the “sample information edit” button 55 is instructed, a sample information edit screen shown in FIG. 7 to be described later is displayed.

  FIG. 6 is a screen diagram illustrating an example of a screen displayed on the display 37. The screen 60 is a screen for displaying information on liquid volume management. The remaining amounts of the six eluent containers are displayed in the display windows B1 to B6, and the remaining amounts of the three reaction reagent containers are displayed in the display windows R1 to R3. In addition, the remaining amount of the cleaning liquid container is displayed on the cleaning liquid display window, and the amount of the remaining liquid in the waste liquid container is displayed on the waste liquid display window. This display allows the user to know the current amount of liquid in each container. When the “close” button 61 is designated, the screen returns to the screen 50 shown in FIG. When the “sample information editing” button 62 is designated, a sample information editing screen is displayed.

  FIG. 7 is a screen diagram showing an example of a screen displayed on the display 37, and shows an example of a sample information editing screen. In the sample information editing screen, the sample information when the continuous analysis is executed is displayed in a table format. The screen 70 displays a sample table 71 when the user designates analysis contents when executing continuous analysis on seven types of samples.

  In the sample table 71, the order of analysis is arranged vertically, and the contents of each analysis can be displayed in default or input. In the example of FIG. 7, there are seven containers or vials containing samples, the amount per injection into the diluent prepared in advance, the number of injections into the diluent, the type of sample, the type of diluent The dilution factor, the name of the sample, and the file name defining the analysis conditions defined for each sample are displayed. The types include a standard sample described as “STD” in FIG. 7 and an analysis target sample whose component is described as “UNK”. In addition to the input of these items, it is possible to insert a new line or delete a line. The contents of the sample table 71 do not need to be entered entirely by the user. When the minimum specific information such as the number of specimens and the analysis method is entered, the control unit 15 automatically creates the sample table. The user can check and edit the automatically generated sample table.

  The storage unit 39 stores a flow rate program for predicting the amount of reagent used, and the amount of reagent used is predicted based on the analysis conditions set in the sample table 71. When the user confirms or rewrites the data used in the flow program, when the “edit flow program” button 72 in FIG. 7 is instructed, a screen for editing the flow program is displayed.

  FIG. 8 is a screen diagram showing a screen for editing the flow program, and is a screen showing an example of data used in the flow program in one analysis. As shown in FIG. 8A, the contents of the data are “TIME” indicating the elapsed time from the left, the mixing ratio “% B” of the eluent with respect to the flow rate, the flow rate “FLOW1” at the elapsed time, and the like. In an example of the data table 81 displayed on the screen 80 shown in FIG. 8B, the ratio “% R” of the reaction reagent with respect to the flow rate and the flow rate corresponding thereto are also displayed. In accordance with the data stored in the data table 81, the control unit 15 controls the flow rate, the ratio of the eluent to the flow rate, and the ratio of the reaction reagent to the flow rate.

  FIG. 9 is a screen diagram displaying a calculation formula for predicting the consumption amount of a reagent such as an eluent or a reaction reagent, and the result. “I” is from 1 to n, t0 is the analysis start time, and tn is the analysis end time. “J” indicates the vial number. The calculation formula is to obtain the consumption Vj for the reagent Bj, where ti is the elapsed time, B is the mixing ratio of the sample to the reagent, and F is the flow rate sent by the pump.

  FIG. 9B shows an example of calculation by applying the data shown in FIG. 8 to this calculation formula. The expected reagent consumption is displayed on the screen 90. The expected reagent consumption from the multiple injection analysis designations to the end of the analysis process in the analysis process set in the sample table of FIG. 7 is the sum of the reagent consumptions per injection analysis. In the example of the figure, it can be seen that the eluent B2 and the reaction reagent R2 are “20 ml”, which is larger than the others. It can also be seen that the amount of waste liquid is “110 ml”. When the “Calculate” button 91 in the screen 90 is instructed, a screen indicating what the reagent amount in the container is calculated from the current reagent amount is displayed.

  FIG. 10 is a screen diagram showing an example of a screen that displays a value obtained by subtracting the estimated reagent consumption from the detected current reagent remaining amount. The amount of waste liquid is the current amount plus the expected amount. On the screen 100 shown in FIG. 10, the eluent of B1 is displayed as “−150 ml”, indicating that 150 ml is insufficient. The reaction reagent for R1 is also displayed as “−150 ml”, indicating that 150 ml is insufficient. Since the sampler cleaning solution is “50 ml”, it can be seen that 50 ml remains. The waste liquid is displayed as “9999 ml” instead of a specific number, indicating that it overflows. Here, the overflow may be displayed, or specifically, how much the overflow will be displayed. In addition, when the estimated reagent consumption amount is larger than the current reagent amount compared to the current reagent remaining amount, not only a minus display but also a display of the expected reagent consumption amount of the reagent, for example, can be seen at a glance. For the reagent container image displayed in red letters or displayed on the screen at the same time, the effect of prompting the replacement of the container can be obtained by displaying a warning such as displaying the corresponding container in red. .

  In addition, in order to prevent the analysis from being started even though it is predicted that the reagent is insufficient, the screen 100 includes a “add / discard liquid” button 101 and a “reduce the total number of samples” button 102. Is displayed so that only one of the following processes can be selected.

  FIG. 11 is a message screen displayed when the “add / discard liquid” button 101 is instructed in FIG. Since the message displayed on the screen 110 indicates what and how much is added, the user adds a reagent or replaces the container according to this message. In the example shown, it is instructed to exchange a 250 milliliter B1 container and a 500 milliliter R1 container.

  When the user designates the “work end” button 111 after the maintenance work is completed, the reagent amount in the replaced container is detected, the expected reagent consumption amount is calculated, and the screen shown in FIG. 10 is displayed again with a new value. Is done. When the current reagent remaining amount becomes larger than the expected reagent consumption, it is possible to move to the next analysis step.

  In the screen shown in FIG. 10, when the user designates the “decrease total number of samples” button 102, the sample table shown in FIG. 7 is displayed. By saving the table, the reagent amount in the container is detected and the estimated reagent consumption amount is calculated again, and the screens shown in FIGS. 9 and 10 are displayed.

  FIG. 12 is a screen diagram illustrating an example of a message screen. In the screen shown in FIG. 10, the user designates the “reduce total sample number” button 102, edits the sample table shown in FIG. 7 to reduce the number of samples, and saves the sample table. Detection of reagent amount and calculation of expected reagent consumption are performed. As a result, the screens shown in FIGS. 9 and 10 are displayed.

  The next process is not executed until the current reagent remaining amount becomes larger than the expected reagent consumption. When the sample table shown in FIG. 7 is re-edited during the analysis step (4) shown in FIG. 2, the reagent container is measured and the estimated reagent consumption is calculated. When it is determined that the amount is smaller than the expected amount of reagent consumption in the future, an operation guidance screen shown in FIG. 12 is displayed, and guidance for urging reagent maintenance work after the analysis process is stopped is displayed. When the “Close” button is instructed, the reagent and waste liquid management start screen shown in FIG. 5 is displayed.

  Next, management of the amount of waste liquid will be described. The amino acid analyzer of the present invention has a waste liquid amount measuring device for informing the current waste liquid amount, an input device and a calculation function for inputting the number of samples and the waste liquid amount per sample, and an output function for notifying a user of a warning. Have.

  FIG. 13 is a configuration diagram showing an outline of a system for detecting the liquid amount in the container 131. By providing the system shown in FIG. 13 in an amino acid analyzer or a liquid chromatograph, a “waste liquid amount warning” can be performed.

  The waste liquid amount measuring device includes a container 131 having RFID tags 130a to 130j instead of scales on the side of the container, and a read / write device 132 that controls reading and writing of data by wireless communication with the RFID tags 130a to 130j. Yes. The number of RFID tags varies depending on the container capacity. Each RFID tag 130a to 130j stores a scale position of the tag and communication date / time information. The control unit 15 is provided with a communication control unit 33 that controls reading and writing of this information, and transmits radio waves to all RFID tags via the read / write device 132.

  As the container 131, usually only one container with a large capacity is prepared, and when an RFID tag is provided in the container 131, the amount of waste liquid increases, so it is necessary to monitor so as not to overflow. The amount of waste liquid accumulated in the container 131 is detected by a plurality of RFID tags, the amount of waste liquid generated by the execution of the analysis is predicted and calculated, and whether or not the remaining capacity of the container 131 overflows is calculated before analysis. The message is displayed on the display 37. When the capacity is insufficient as a result of the prediction calculation, a message is displayed to the user to prepare a new container before analysis, and the waste liquid is prevented from spilling from the container 131.

  In the example of FIG. 13, when the RFID tag 130a is the RFID tag at the highest position and the read / write device 132 cannot detect the RFID tag 130a, the information analysis unit 34 determines that the free capacity of the container 131 is close to zero. Then, the communication date and time and the ID of the container 131 are transmitted to the calculation unit 35 of the control unit 15. The computing unit 35 causes the display 37 to display a message indicating that the amount of waste liquid in the container 131 is close to overflow with an image in a pre-programmed format via the input / output unit 36. A user who sees a message that the amount of waste liquid is close to overflow inputs a signal indicating confirmation from an input device 38 such as a mouse or keyboard of a personal computer.

  When the read / write device 32 no longer detects the RFID tag 130a at the highest position of the container 131 shown in FIG. 13, the free capacity is close to zero, and no further analysis can be performed. At the time of analysis, since the amount of waste liquid can be calculated from the flow program shown in FIG. 8, it communicated with any one of the plurality of RFID tags 130a, 130b,... 130j attached to the container 131 shown in FIG. By adding the amount of waste liquid that can be determined by the above and the predicted value of the amount of waste liquid generated, it can be determined whether it is necessary to prepare another waste liquid container. In this manner, by managing the amount of waste liquid in the container 131 by using a plurality of RFID tags attached to the container 131, it is possible to avoid interruption of analysis due to overflow of the waste liquid during analysis.

  FIG. 14 is a flowchart illustrating waste liquid amount measurement processing in the information analysis unit. First, communication is performed with all RFID tags to acquire information (step 1401). The communication results are checked in order from the uppermost RFID tag 130a attached to the side surface of the container 131 (step 1402). There is no waste liquid at the position of the RFID tag that can communicate, and there is waste liquid at the position of the RFID tag that cannot communicate. By detecting the boundary between communicable and incapable communication, the current amount of waste liquid in the waste liquid container can be known (step 1403).

  Normally, since the amount of waste liquid increases, it is possible to manage the amount of waste liquid by monitoring which RFID tag can communicate and storing the amount of waste liquid in the storage unit 39. If the amount of waste liquid in the container 131 has decreased as compared with the previous information, it indicates that the waste liquid has been disposed of by the user, so the amount of waste liquid stored in the storage unit 39 is rewritten. .

  FIG. 15 is a message screen displayed when the “add / dispose liquid” button in FIG. 10 is instructed. A message shown on the screen 150 is displayed when the waste liquid is close to overflow. The user disposes of the waste liquid in the container according to the guidance, executes the maintenance work to attach the empty container, and instructs the “end work” button 151 to again measure the waste liquid amount of the waste liquid container and calculate the expected total waste liquid amount. Is done. The next step is not executed until the sum of the current waste liquid amount and the expected total waste liquid amount is smaller than the allowable amount of the waste liquid container. When there is also a shortage of eluent or reagent shown in FIG. 11, the message shown in FIG. 11 and the message shown in FIG. 15 are displayed simultaneously.

  FIG. 16 is a screen diagram illustrating an example of a message screen. In the screen shown in FIG. 10, the user designates the “reduce total sample number” button 102, edits the sample table shown in FIG. 7 to reduce the number of samples, and saves the sample table. And the expected amount of waste liquid is calculated. As a result, the screen shown in FIG. 15 is displayed. If the free capacity of the current waste liquid container is not larger than the expected amount, the next step is not executed. 2 is re-edited during the analysis step (4) shown in FIG. 2, the amount of waste liquid is measured and the expected amount of waste liquid is calculated. As a result, the current waste container When it is determined that the available capacity is smaller than the expected amount of waste liquid in the future, the operation guidance screen shown in FIG. 16 is displayed, and guidance for prompting maintenance work of waste liquid disposal is displayed after the analysis process is stopped. When the “Close” button is instructed, the reagent and waste liquid management start screen shown in FIG. 5 is displayed.

  The liquid chromatograph apparatus of the above-described embodiment of the present invention includes an RFID tag read / write device that communicates with an RFID tag of a container having a plurality of RFID tags, and knows the amount of liquid by communicating with the RFID tag. And a function of reading the type of reagent and writing the read date and time to the RFID tag.

  In addition, as an analysis condition, an input device in which the user inputs in advance the number of samples and the amount of reagent used per sample, and a control unit having a calculation unit for predicting and calculating the amount of reagent necessary for the execution of analysis and the amount of waste liquid generated And an output device that notifies the user of the amount of reagent before and after analysis, the amount of waste liquid, or the presence or absence of overflow.

  As described above, according to the embodiment of the present invention, the amount of liquid in the reagent container and the waste liquid container can be accurately grasped and managed without visual observation by the user. A message prompting the user to replenish the reagent or dispose of the waste liquid is displayed on the display by predicting the amount of reagent used and the amount of waste liquid generated by the analysis. As a result, the analysis of amino acid analyzers and liquid chromatographs can be prevented from being interrupted due to reagent shortage or waste liquid overflow, and reagent replenishment and waste liquid treatment can be performed at an appropriate time. An apparatus and a liquid chromatograph apparatus can be obtained.

DESCRIPTION OF SYMBOLS 1 Eluent pump 2 Reaction reagent pump 3 Eluent container 4 Nitrogen gas container 5 Regeneration liquid container 6 Reaction reagent container 7 Reaction system washing | cleaning liquid container 8 Ammonia filter column 9 Autosampler 10 Separation column thermostat 11 Separation column 12 Reaction apparatus 13 Reaction column 14 Visible detector 15 Control unit 16 Waste liquid container 31 Containers 32, 132 Read / write device 33 Communication control unit 34 Information analysis unit 35 Calculation unit 36 Input / output unit 37 Display 38 Input device 39 Storage unit 131 Container

Claims (9)

In a liquid chromatograph that separates a sample into components using a separation column and detects the separated components,
A reagent container for storing a reagent for feeding or reacting the specimen, a read / write device for detecting the amount of liquid in the container by providing a plurality of RFID tags in a waste liquid container for storing waste liquid after component detection;
Based on the number of samples and the amount of reagent used per sample, the total amount of reagent used and the amount of waste liquid generated are predicted. If the reagent in the reagent container is insufficient, an insufficient message is displayed on the display device. A liquid chromatograph apparatus comprising: a calculation unit that displays an overflow message on a display device when the waste liquid container overflows. A read / write device that communicates with the RFID tag of an eluent container having a plurality of RFID tags;
An information analysis unit that reads the amount and type of the eluent in the eluent container by communication with the RFID tag, and writes the read date and time to the RFID tag,
A separation column for separating the sample to be analyzed injected into the eluent into components;
A detection unit for detecting a component of the sample separated by the separation column;
The amount of the eluent used is predicted based on the type of the sample and the type of the eluent, and the eluent in the eluent container is determined from the amount of the eluent in the eluent container and the predicted amount used. A liquid chromatograph apparatus comprising: a calculation unit that calculates a remaining amount of the liquid crystal and displays a shortage on the display device when the eluent in the eluent container is insufficient.   3. The liquid chromatograph device according to claim 2, wherein the RFID tag is provided along a direction in which the liquid level of the eluent on the outer surface of the eluent container increases or decreases. The second read / write device according to claim 2, wherein the second read / write device communicates with the RFID tag of a waste liquid container having a plurality of RFID tags.
The information analysis unit reads the amount of waste liquid in the waste liquid container by communication with the RFID tag and writes the read date and time to the RFID tag.
The calculation unit predicts the generation amount of the waste liquid based on the type of the sample and the type of the eluent, and the waste liquid in the waste liquid container from the amount of the waste liquid in the waste liquid container and the predicted generation amount A liquid chromatograph apparatus characterized in that when the amount of the waste liquid in the waste liquid container overflows, the overflow is displayed on the display device.   5. The liquid chromatograph according to claim 4, wherein the RFID tag is provided along a direction in which the liquid level of the waste liquid on the outer surface of the waste liquid container increases or decreases. The reaction column according to claim 2, wherein the sample in the eluent mixed with the reaction reagent is reacted with the reaction reagent;
A third read / write device in which the reaction reagent is stored and communicating with the RFID tag of a container having a plurality of RFID tags;
The calculation unit predicts the usage amount of the reaction reagent based on the type of the sample and the type of the reaction reagent, and the container is calculated from the amount of the reaction reagent in the container and the usage amount predicted by the calculation unit. A liquid chromatograph apparatus characterized in that a remaining amount of a reaction reagent in the container is obtained, and when the reaction reagent in the container is insufficient, a shortage is displayed on a display device.   7. The liquid chromatograph device according to claim 6, wherein the RFID tag is provided along a direction in which the liquid level of the reaction reagent on the outer surface of the container increases or decreases.   The calculation unit according to claim 6, wherein the calculation unit predicts the amount of the waste liquid generated based on the type of the sample, the type of the eluent, and the type of the reaction reagent, and the amount of the waste liquid in the waste liquid container An amount of waste liquid in the waste liquid container is obtained from the predicted generation amount, and when the waste liquid in the waste liquid container overflows, the liquid chromatograph apparatus displays the overflow on the display device. A method for managing a liquid chromatograph device in which a sample is injected into an eluent and separated into components by a separation column, and the components are detected by a detection unit,
Obtaining the amount of the eluent by communicating with a plurality of RFID tags provided on the side surface of the eluent container containing the eluent,
Obtaining the amount of the waste liquid by communicating with a plurality of RFID tags provided on the side surface of the waste liquid container for storing the waste liquid after component detection in the detection unit,
A sample table in which information for executing a continuous analysis set from analysis conditions selected from analysis conditions set in advance in the storage unit, the sample type, and the number of samples is tabulated is created and stored Stored in the department,
Based on the sample table stored in the storage unit, the use amount of the eluent and the generation amount of waste liquid are calculated,
The remaining amount of the eluent stored in the eluent container is obtained from the amount of the eluent stored in the eluent container and the calculated amount of use of the eluent. Is displayed,
The remaining amount of waste liquid stored in the waste liquid container is obtained from the amount of waste liquid stored in the waste liquid container and the calculated amount of generated waste liquid, and an overflow message is displayed on the display device in case of overflow. A method for managing a liquid chromatograph apparatus.

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