Chromatograph device and method for setting sample introduction amount

Abstract

In this invention, a test processing unit 102 carries out a plurality of test analyses with different sample introduction amounts into a separation column 36 in a prescribed order corresponding to the introduction amounts. A determination processing unit 104 determines whether to make the test processing unit 102 carry out the next test analysis according to the prescribed order on the basis of a detection result of a detection unit 38 at the time of test analysis. If the determination processing unit 104 determines not to carry out the next test analysis, an introduction amount setting processing unit 116 sets a repeat introduction amount on the basis of the sample introduction amount at the time of completed test analysis. A repeat introduction processing unit 108 repeatedly carries out introduction processing for introducing the repeat introduction amount of the sample into the separation column 36.

Description

[Technical field]

[0001] The present invention relates to a chromatographic device and a method for setting a sample introduction amount. [Background technology]

[0002] For example, in a conventional chromatographic device such as that disclosed in Patent Document 1 below, a mobile phase is introduced into a column together with a sample, and components in the sample separated in the column are detected in a detection section.

[0003] In a liquid chromatograph, which is an example of a chromatographic device, a sample is introduced into a column together with a liquid mobile phase. The amount of sample introduced into the column is set according to the concentration of components in the sample and the responsiveness of the detection unit. In addition, when performing preparative separation and purification, the amount of sample introduced into the column is set according to the required amount of purification. [Prior art documents] [Patent documents]

[0004] [Patent Document 1] International Publication No. 2017 / 208300 Summary of the Invention [Problem to be solved by the invention]

[0005] However, if the amount of sample introduced into the column is excessive, the amount of components in the sample that can be retained in the column may be exceeded, and the retention sites in the column may be exhausted. In this case, the peak shape and resolution of the components in the sample detected in the detection unit may deteriorate, and analysis or fractionation may not be performed well. In addition, when a large amount of sample is introduced, the sample solvent behaves like a mobile phase, so if the elution power of the sample solvent is strong, the band width of the components in the sample may widen, and the peak shape and resolution may deteriorate. On the other hand, if the amount of sample introduced is insufficient, the peak shape and resolution may not be a problem, but the detection sensitivity may be insufficient, and quantitative analysis such as concentration may not be performed accurately. These problems are not limited to when the mobile phase is liquid, but can also occur when the mobile phase is gas.

[0006] The present invention has been made in view of the above-mentioned circumstances, and aims to provide a chromatographic apparatus and a method for setting a sample introduction amount that can set an appropriate amount of sample to be introduced into a column. Another aim of the present invention is to provide a chromatographic apparatus and a method for setting a sample introduction amount that does not require an analyst to consider the amount of sample to be introduced into a column. Another aim of the present invention is to provide a chromatographic apparatus and a method for setting a sample introduction amount that can prevent the time and results of considering the amount of sample to be introduced into a column from differing depending on the analyst. [Means for solving the problem]

[0007] A first aspect of the present invention is a chromatographic device that introduces a mobile phase into a column together with a sample and detects components in the sample separated in the column with a detection unit, and includes a test processing unit, a determination processing unit, an introduction amount setting processing unit, and a repetitive introduction processing unit. The test processing unit performs multiple test analyses with different amounts of sample introduced into the column in a predetermined order according to the introduction amounts. The determination processing unit determines whether or not to perform a next test analysis in the test processing unit according to the predetermined order based on a detection result by the detection unit during a test analysis. When the determination processing unit determines that a next test analysis is not to be performed, the introduction amount setting processing unit sets a repetitive introduction amount based on the introduction amount of sample during a previously performed test analysis. The repetitive introduction processing unit repeats an introduction process of introducing a sample into the column with the repetitive introduction amount multiple times.

[0008] A second aspect of the present invention is a method for setting an amount of sample to be introduced into a chromatographic device, which introduces a mobile phase into a column together with a sample and detects components in the sample separated in the column with a detection unit, and includes a test step, a judgment step, and an introduction amount setting step. In the test step, multiple test analyses with different amounts of sample introduced into the column are performed in a predetermined order according to the introduction amounts. In the judgment step, it is judged whether or not to perform a next test analysis in the test step according to the predetermined order based on a detection result by the detection unit during the test analysis. In the introduction amount setting step, when it is judged in the judgment step that a next test analysis will not be performed, an introduction amount to be repeated when an introduction process of introducing a sample into the column in the chromatographic device is repeated multiple times is set based on the amount of sample introduced during the previously performed test analysis. Effect of the Invention

[0009] According to the present invention, the amount of sample introduced into the column can be set to an appropriate value. Also, according to the present invention, the analyst does not need to consider the amount of sample introduced into the column. Furthermore, according to the present invention, the amount of sample introduced into the column can be prevented from differing depending on the analyst. [Brief description of the drawings]

[0010] [Figure 1] 1 is a block diagram showing an example of the overall configuration of a chromatographic device according to a first embodiment. [Diagram 2] FIG. 4 is a diagram for explaining an example of an automatic setting process according to the first embodiment. [Diagram 3] FIG. 2 is an illustrative view showing an example of a memory map of a RAM in the first embodiment; [Figure 4] FIG. 2 is a block diagram showing an example of a functional configuration of the chromatographic device of the first embodiment. [Diagram 5] FIG. 4 is a flowchart showing an example of operation processing of a CPU of the chromatographic device of the first embodiment. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0011] 1. Overall configuration of the chromatography device 1 is a block diagram showing an example of the overall configuration of a chromatographic device 10 according to the first embodiment. In the first embodiment, the chromatographic device 10 will be described by taking a liquid chromatographic device as an example.

[0012] The chromatographic apparatus 10 includes a control unit 20, a mobile phase container 28, a liquid delivery pump 30, a sample introduction unit 32, a column oven 34, a separation column 36, a detection unit 38, a signal processing circuit 40, a switching unit 42, a fractionation unit 44, a display unit 46, a display control circuit 48, an operation unit 50, and an operation detection circuit 52. The control unit 20 also includes a CPU (Central Processing Unit) 22. The control unit 20 also includes a RAM (Random Access Memory) 24 and a storage unit 26 that are directly accessible by the CPU 22.

[0013] The control unit 20 is electrically connected to each of the liquid delivery pump 30, the sample introduction unit 32, the column oven 34, the signal processing circuit 40, the switching unit 42, the fraction collection unit 44, the display control circuit 48, and the operation detection circuit 52 via a connection circuit 54 such as a bus. In addition, the signal processing circuit 40 is electrically connected to the detection unit 38, the display control circuit 48 is electrically connected to the display unit 46, and the operation detection circuit 52 is electrically connected to the operation unit 50.

[0014] The control unit 20 is responsible for overall control of the chromatographic device 10. The CPU 22 controls each component of the chromatographic device 10. The RAM 24 is used as a work area and a buffer area for the CPU 22. The storage unit 26 is a non-volatile memory, and for example, a hard disk drive (HDD) or a solid state drive (SSD) is used as the storage unit 26.

[0015] The storage unit 26 stores a control program for controlling each component of the chromatographic device 10, data required for executing the control program (execution data), etc. The storage unit 26 may be configured to include the RAM 24.

[0016] The mobile phase container 28 is a container for storing the mobile phase, and the liquid delivery pump 30 is a pump for delivering the mobile phase. During analysis, the liquid delivery pump 30 delivers the mobile phase continuously at a constant speed. The sample introduction section 32 is a general-purpose sample introduction device such as an autosampler, and the column oven 34 is a general-purpose heating device for heating the separation column 36 therein.

[0017] The detection unit 38 is a general-purpose detection device that detects components in the sample separated by the separation column 36. The signal processing circuit 40 amplifies the signal output from the detection unit 38, performs A / D (analog / digital) conversion on the signal, and outputs the signal to the control unit 20.

[0018] The switching unit 42 is provided to switch the introduction destination of the sample after it has been introduced into the detection unit 38 between the fraction collection unit 44 and an outlet (not shown). The switching unit 42 includes, for example, a general-purpose three-way valve. When the introduction destination of the sample is set to the fraction collection unit 44 by the switching unit 42, the sample is introduced into the fraction collection unit 44. When the introduction destination of the sample is set to the outlet, the sample is discharged from the outlet. However, the configuration may be such that only fraction collection can be performed by omitting the switching unit 42.

[0019] The fraction collection section 44 includes, for example, a general-purpose fractionation device that collects components separated by the separation column 36. The sample after the various components are collected by the fraction collection section 44 is discharged from an outlet (not shown). However, the fraction collection section 44 may be omitted so that only analysis can be performed.

[0020] The display unit 46 is a general-purpose display device such as an LCD (Liquid crystal display) or an EL (Electro-Luminescence) display. The display control circuit 48 includes a GPU, a VRAM, and the like. Under the instruction of the CPU 22, the GPU generates display images in the VRAM for displaying various screens on the display unit 46 using image generation data stored in the RAM 24, and outputs a display image corresponding to the display image data to the display unit 46.

[0021] The operation unit 50 includes hardware keys (operation keys) of the chromatographic device 10. Examples of the operation keys include a power key. The operation unit 50 also includes an input device. Examples of the input device include a keyboard and a mouse. The input device may also include a touch panel. In this case, the touch panel is provided on the display surface of the display unit 46. A touch panel display in which the touch panel and the display are integrally formed may also be used. The operation detection circuit 52 outputs a signal or operation data corresponding to the operation of the operation unit 50 to the control unit 20.

[0022] In such a chromatographic apparatus 10, various components are controlled by the control unit 20, and the mobile phase is delivered from the mobile phase container 28 by the operation of the liquid delivery pump 30. When the mobile phase is delivered from the mobile phase container 28, the sample introduction unit 32 introduces the sample into the mobile phase. After the sample is introduced, components in the sample are separated in the separation column 36, and the sample is introduced into the detection unit 38. The sample components separated into individual components are detected in the detection unit 38. If necessary, the components separated by the separation column 36 are introduced into the fractionation unit 44, and the various components are fractionated in the fractionation unit 44.

[0023] Therefore, such a chromatographic apparatus 10 can perform a process (introduction process) of introducing a sample into the separation column 36. The introduction process can be performed, for example, in an analysis process for analyzing components contained in the sample, or in a fractionation process for fractionating components contained in the sample.

[0024] 2. Overview of the automatic configuration process In the chromatographic device 10 of the first embodiment, when a predetermined operation is detected, an automatic setting process is executed. In addition, when the automatic setting process is executed, an introduction process is repeatedly executed according to the setting items that are set in association with the execution of the automatic setting process.

[0025] That is, the automatic setting process in the first embodiment is a process for setting setting items (repeated setting items) related to the repeated introduction process after the automatic setting process.

[0026] The repetition setting items include the amount of sample introduced into the separation column 36 in the repeated introduction process (repetition introduction amount) and the number of times the introduction process is repeated (repetition number).

[0027] As will be described in detail later, in the automatic setting process, a test analysis of a sample is performed multiple times. Furthermore, in the multiple test analyses, the amount of sample introduced into the separation column 36 is different for each.

[0028] That is, in the automatic setting process, multiple test analyses are performed in which the amount of sample introduced into the separation column 36 is different, and the setting items are set repeatedly.

[0029] In the following, the amount of sample introduced in each test analysis will be simply referred to as a “test amount.” First, a series of processes up to the execution of the automatic setting process will be described.

[0030] Although not shown in the figures, in the first embodiment, for example, when a specific icon is operated while the main menu screen of the chromatographic device 10 is displayed on the display unit 46, a screen (execution screen) for executing the automatic setting process is displayed on the display unit 46.

[0031] On the execution screen, setting items (test setting items) related to multiple test analyses are appropriately set by operating icons provided on the execution screen.

[0032] The test setting items include, for example, a test amount, a test order, etc. A plurality of test amounts are set according to the number of times the test analysis is repeatedly performed. However, the plurality of test amounts may be preset as default values.

[0033] The test order sets the order in which multiple test analyses are performed. The test analysis order is set in ascending order in which the test amount is gradually increased, or in descending order in which the test amount is gradually decreased. When the test analysis order is set to ascending order, the multiple test analyses are performed in an order according to the ascending order of the test amount, and when the test analysis order is set to descending order, the multiple test analyses are performed in an order according to the descending order of the test amount. However, the test analysis order may be automatically selected depending on the type of introduction process that is repeatedly executed after the automatic setting process.

[0034] The types of introduction processes repeatedly performed after the automatic setting process include a large amount introduction, which is set so that the amount of sample introduced into the separation column 36 in one introduction process is as large as possible, and a small amount introduction, which is set so that the amount of sample introduced into the separation column 36 in one introduction process is as small as possible. When fractionation is performed in the fractionation unit 44, it is preferable to select a large amount introduction in order to reduce the number of times the introduction process is repeatedly performed until a predetermined amount of sample components is fractionated, and to efficiently fractionate the components in the sample. On the other hand, when components contained in a small amount of sample are detected by the detection unit 38 (high sensitivity analysis), it is preferable to select a small amount introduction in order to minimize the amount of sample used. Although a detailed description is omitted, even in the case of a large amount introduction, an upper limit is set for the amount of introduction based on the performance of the components constituting the chromatographic device 10.

[0035] When a large amount is introduced, the test analyses performed in advance are performed in ascending order, so that the amount of repeated introduction during the repeated introduction process is set to as large a value as possible. On the other hand, when a small amount is introduced, the test analyses performed in advance are performed in descending order, so that the amount of repeated introduction during the repeated introduction process is set to as small a value as possible. In each test analysis, whether or not to perform the next test analysis is determined based on whether an index related to the peak of the chromatogram (peak index) is equal to or greater than a threshold value, or whether the peak index is less than a threshold value.

[0036] Examples of the peak index include an index based on the degree of peak resolution, an index based on the intensity of the peak, etc. The index based on the degree of peak resolution is an index that indicates the state of separation between peaks, and is calculated based on the number of theoretical plates that indicates the performance of the separation column 36. Examples of the index based on the intensity of the peak include the height of the peak, the area of ​​the peak, and the signal-to-noise (SN) ratio.

[0037] In the first embodiment, for example, when an icon to which a function for executing an automatic setting process is assigned is operated while the execution screen is displayed on the display unit 46, the automatic setting process is started. Note that the method of setting the test setting items and the method of executing the automatic setting process are merely examples and are not particularly limited.

[0038] 3. Details of the automatic configuration process In the first embodiment, when the automatic setting process is executed, the test setting items are referenced, and multiple test analyses each having a different test amount are executed in ascending or descending order of the test amount as described above.

[0039] Fig. 2 is a diagram for explaining an example of the automatic setting process of the first embodiment. In the example shown in Fig. 2, a first test amount to an n-th test amount are set in advance. Note that n is a variable, and in the example shown in Fig. 2, n is a value of 4 or more. Hereinafter, the automatic setting process will be specifically described with reference to Fig. 2.

[0040] In the automatic setting process, each time a test analysis is performed, a determination is made as to whether or not to perform a next test analysis based on the detection result of the test analysis. Specifically, the determination as to whether or not to perform a next test analysis is made by referring to the chromatogram in the test analysis and comparing the peak index with a threshold value.

[0041] For example, when the test analysis is performed in ascending order and an index based on the separation degree of the peaks is compared with a threshold value as a peak index, if the analysis result of the test analysis shows that the peak index is equal to or greater than the threshold value, the next test analysis is performed, and if the peak index is less than the threshold value, the next test analysis is not performed. When the test analysis is performed in descending order and an index based on the intensity of the peaks is compared with a threshold value as a peak index, if the analysis result of the test analysis shows that the peak index is less than the threshold value, the next test analysis is performed, and if the peak index is equal to or greater than the threshold value, the next test analysis is not performed. Note that if it is determined that the next test analysis is not to be performed, the remaining test analyses are not performed.

[0042] Furthermore, in the automatic setting process, when it is determined that the next test analysis is not to be performed, the repeat introduction amount is set based on the test amount in the previously performed test analysis.

[0043] For example, one of the test amounts in the test analysis that has already been performed is set as the repeat introduction amount. As shown in FIG. 2, it is preferable that the test amount in the test analysis immediately before when it is determined that the next test analysis is not to be performed is set as the repeat introduction amount.

[0044] In the example shown in FIG. 2, after test analyses are performed in the order of the first test amount, the second test amount, and the third test amount, if it is determined that the next test analysis will not be performed, the second test amount is set as the repeated introduction amount.

[0045] However, if it is determined during the first test analysis (test analysis with the first test amount) of the multiple test analyses that the next test analysis is not to be performed, the repeat introduction amount is not set. In this case, the remaining test analyses are not performed, and the subsequent repeat introduction processes are not performed either.

[0046] Although not shown in the figures, when it is determined during the first test analysis of the multiple test analyses that the next test analysis will not be performed, a notification may be issued to prompt the user to reset the test amount. For example, a message prompting the user to reset the test amount may be displayed on the display unit 46. In this case, for example, an execution screen may be displayed again on the display unit 46.

[0047] Furthermore, in the last test analysis of the multiple test analyses, if it is determined that the next test analysis should be performed, instead of performing the test analysis, the repeat introduction amount is set based on the test amount in the previously performed test analysis, as described above.

[0048] When the last test analysis is performed and it is determined that the next test analysis should be performed, it is preferable that the test amount in the last test analysis is set as the repeat introduction amount. In the example shown in Figure 2, when the test analysis with the nth test amount is performed and it is determined that the next test analysis should be performed, the nth test amount is set as the repeat introduction amount.

[0049] In the first embodiment, when the amount of repeated introduction is set, the number of repetitions is set based on the amount of repeated introduction. Specifically, when the number of repetitions is set, the remaining amount of sample to be used is calculated. When the remaining amount of sample is calculated, the remaining amount is divided by the amount of sample to be used in one sample introduction corresponding to the amount of repeated introduction, and the quotient is set as the number of repetitions.

[0050] For example, when it is determined that the next test analysis will not be performed and the test amount from the previous test analysis is set as the amount introduced repeatedly, the remaining amount of sample to be used is expressed by the following formula 1. On the other hand, when it is determined in the last test analysis that the next test analysis will be performed and the last test amount is set as the amount introduced repeatedly, the remaining amount of sample to be used is expressed by the following formula 2. Note that in formulas 1 and 2, the left side indicates the remaining amount of sample immediately after the automatic setting process is performed. In other words, the right side indicates the total amount of sample before the automatic setting process is performed minus the amount of sample used by the test analysis. The total amount of sample may be stored in advance in memory unit 26.

number

number

[0051] The number of repetitions is expressed by the following formula 3. In formula 3, the left side indicates the number of repetitions. In other words, the right side indicates that the remaining amount of sample immediately after the automatic setting process is performed is divided by the amount of sample used in one sample introduction corresponding to the repeated introduction amount.

number

[0052] However, if the remaining amount of sample immediately after the automatic setting process is executed is less than the amount of sample used in one sample introduction corresponding to the repeated introduction amount, a shortage of sample may be notified.

[0053] The number of times the introduction process is repeated is set by the above calculation, but if a remainder is calculated as a result of the calculation of Equation 3, an additional process is performed to introduce the sample because there is less sample left for one run. In this case, the number of times the introduction process is performed is one more than the number calculated by Equation 3.

[0054] For these reasons, in the first embodiment, if it is determined in a test analysis other than the first test analysis that the next test analysis will not be performed, and if it is determined in the last test analysis that the next test analysis will be performed, a repeat setting item is set, and the introduction process is repeatedly executed according to that repeat setting item.

[0055] Furthermore, when it is determined in the test analysis that a next test analysis should be performed, the components separated in the separation column 36 during the test analysis may be fractionated in the fractionation section 44. In this case, fractionation of the components in the sample is possible even during the test analysis, and unnecessary consumption of the sample can be suppressed.

[0056] 4. Programs and Data 3 is a schematic diagram showing an example of a memory map 200 of the RAM 24 in the first embodiment. As shown in the figure, the RAM 24 includes a program area 201 and a data area 202. In the program area 201, a control program previously read out from the storage unit 26 is stored.

[0057] The control programs include an image generating program 201a, a display program 201b, an operation detecting program 201c, an operation controlling program 201d, a test program 201e, a determining program 201f, a setting program 201g, and a repeat introduction program 201k.

[0058] The setting program 201g includes an introduction amount setting program 201h and a number setting program 201i.

[0059] Image generation program 201a is a program for generating display image data using image generation data 202a, which will be described later.

[0060] The display program 201b is a program for displaying, on the display unit 46, a display image corresponding to the display image data generated according to the image generating program 201a.

[0061] The operation detection program 201c is a program for detecting an operation on the operation unit 50. The CPU 22 stores operation data 202b, which will be described later, in the RAM 24 in chronological order in accordance with the operation detection program 201c.

[0062] The operation control program 201d is a program for controlling various components of the chromatographic apparatus 10. The operation control program 201d includes a program for controlling the liquid delivery pump 30, a program for controlling the sample introduction unit 32, a program for controlling the column oven 34, a program for controlling the detection unit 38 to detect components in the sample, a program for controlling the switching unit 42, and a program for controlling the fractionation unit 44 to fractionate components in the sample.

[0063] The test program 201e is a program for causing the operation control program 201d to execute a plurality of test analyses with different test amounts in a predetermined order according to the test amounts, by referring to the test setting items.

[0064] The judgment program 201f is a program for judging whether or not to execute the next test analysis in the test program 201e, based on the detection result by the detection unit 38 during the test analysis.

[0065] The setting program 201g is a program for setting repetitive setting items when the judgment program 201f judges during a test analysis other than the first test analysis that the next test analysis will not be executed.

[0066] In addition, the setting program 201g is also a program for setting repeated setting items instead of performing the next test analysis with the test program 201e when the judgment program 201f judges that the next test analysis should be performed during the final test analysis among multiple test analyses.

[0067] The introduction amount setting program 201h is a program for repeatedly setting the introduction amount based on the test amount at the time of the executed test analysis.

[0068] The number setting program 201i is a program for, when the amount of repeated introduction is set by the introduction amount setting program 201h, referring to the remaining amount of the sample, and setting the number of repetitions based on the amount of repeated introduction.

[0069] The repeated installation program 201k is a program for repeatedly executing the installation process a plurality of times using the operation control program 201d when a repeated setting item is set by the setting program 201g.

[0070] Although not shown in the figure, other control programs are also stored in the program area 201. For example, a notification program and the like are stored in the program area 201. The notification program is a program for notifying the user of a sample shortage and prompting the user to reset the test amount, etc.

[0071] Data area 202 stores data that has been previously read out from storage unit 26. In the example shown in Fig. 3, data area 202 stores image generation data 202a, operation data 202b, test setting item data 202c, test analysis data 202d, and repeat setting item data 202e.

[0072] Image generation data 202 a is data such as polygon data or texture data for generating display image data corresponding to various screens to be displayed on display unit 46 .

[0073] The operation data 202b is data acquired according to the operation detection program 201c, and is stored in the data area 202 in chronological order.

[0074] The test setting item data 202c is data corresponding to the test setting items, and includes data indicating the test amount and data indicating the test sequence.

[0075] The test analysis data 202d is data showing the result of the test analysis. That is, the test analysis result data 202d is data corresponding to a chromatogram showing the result of the test analysis. Note that the data area 202 may store a plurality of test analysis result data 202d.

[0076] The repeat setting item data 202e is data corresponding to the repeat setting item. The repeat setting item data 202f includes data indicating the repeat introduction amount and data indicating the number of repeats.

[0077] The data area 202 also temporarily stores other execution data and data corresponding to a signal output from the detection unit 38. Furthermore, the data area 202 is provided with a timer (counter) and a register required for executing the control program.

[0078] 5. Functional configuration of the chromatographic device 4 is a block diagram showing an example of a functional configuration of the chromatographic device 10 of the first embodiment. When the CPU 22 executes the operation control program 201d, the control unit 20 functions as an operation control processing unit 100 that controls various components of the chromatographic device 10.

[0079] Furthermore, when the CPU 22 executes the test program 201e, the control unit 20 uses the operation control processing unit 100 to function as a test processing unit 102 that executes multiple test analyses with different test amounts in a predetermined order according to the test amounts.

[0080] Furthermore, when the CPU 22 executes the judgment program 201f, the control unit 20 functions as a judgment processing unit 104 that judges whether or not to cause the test processing unit 102 to execute the next test analysis, based on the detection result by the detection unit 38 during the test analysis.

[0081] Furthermore, during a test analysis other than the first test analysis, if the judgment processing unit 104 determines that the next test analysis will not be performed, when the CPU 22 executes the setting program 201g, the control unit 20 functions as a setting processing unit 106 that sets repeated setting items.

[0082] Also, when the judgment processing unit 104 judges that the next test analysis should be performed during the last test analysis among multiple test analyses, when the CPU 22 executes the setting program 201g, the control unit 20 functions as a setting processing unit 106 that sets the repeat setting items.

[0083] Furthermore, the CPU 22 executes the repetitive introduction program 201k, whereby the control unit 20 uses the operation control processing unit 100 to function as a repetitive introduction processing unit 108 that repeatedly executes the introduction process a plurality of times.

[0084] Furthermore, CPU 22 executes image generation program 201a, thereby functioning as image generation processing unit 110 that generates display image data using image generation data 202a.

[0085] Furthermore, by executing the display program 201b, the CPU 22 functions as a display processing unit 112 that uses the display image data generated by the image generation processing unit 110 to display on the display unit 46 a display image corresponding to the display image data.

[0086] Moreover, the CPU 22 executes the operation detection program 201 c to function as an operation detection processing unit 114 that detects operations on the operation unit 50 .

[0087] The setting processing unit 106 includes an introduction amount setting processing unit 116 that repeatedly sets an introduction amount based on the test amount during the executed test analysis, and this introduction amount setting processing unit 116 corresponds to an introduction amount setting program 201h.

[0088] Furthermore, the setting processing unit 106 includes a number setting processing unit 118 which, when the amount of repeated introduction is set by the introduction amount setting processing unit 116, refers to the remaining amount of sample and sets the number of repetitions based on the amount of repeated introduction, and this number setting processing unit 118 corresponds to the number setting program 201i.

[0089] In the example shown in FIG. 4, for example, when the test processing unit 102 performs multiple test analyses with different test amounts, the judgment processing unit 104 judges whether or not to perform the next test analysis based on the detection result by the detection unit 38 during the test analysis.

[0090] Furthermore, when multiple test analyses are performed, a repeat setting item is set by the setting processing unit 106 as necessary. Furthermore, when a repeat setting item is set, the repeat introduction processing unit 108 repeatedly executes the introduction process multiple times.

[0091] 6. Flow 5 is a flow chart showing an example of the operation process of the CPU 22 of the chromatographic device 10 of the first embodiment. For example, when the CPU 22 detects a predetermined operation, the CPU 22 starts the operation process.

[0092] In step S1, a test analysis is performed, and in step S2, it is determined whether or not to perform the next test analysis. If the answer is "No" in step S2, that is, if the next test analysis is not to be performed, the process proceeds to step S6. On the other hand, if the answer is "Yes" in step S2, that is, if the next test analysis is to be performed, the process proceeds to step S3.

[0093] In step S3, it is determined whether or not the last test analysis has been performed immediately before. If the answer is "No" in step S3, that is, if the last test analysis has not been performed immediately before, the process returns to step S1. On the other hand, if the answer is "Yes" in step S3, that is, if the last test analysis has been performed immediately before, the process proceeds to step S4.

[0094] In step S4, a repeat setting item is set, and in step S5, the introduction process is repeatedly executed a number of times. Also, in step S5, after the introduction process is repeatedly executed, the operation process is terminated.

[0095] In step S6, it is determined whether or not the first test analysis has been performed immediately before. If the answer is "No" in step S6, that is, if the first test analysis has not been performed immediately before, the process proceeds to step S4. On the other hand, if the answer is "Yes" in step S6, that is, if the first test analysis has been performed immediately before, the operation process ends.

[0096] In this way, according to the first embodiment, the analyst can automatically set the amount of sample to be repeatedly introduced to an appropriate value simply by setting the test setting items. Therefore, the analyst does not need to consider the amount of sample to be repeatedly introduced, and the time required to execute the repeated introduction process can be shortened.

[0097] Furthermore, since the repeat setting items are appropriately set simply by setting the test setting items, even if the analyst changes, the repeat setting items are set in the same way as the previous time simply by setting the test setting items in the same way as the previous time. Therefore, the same results can be easily obtained regardless of the analyst.

[0098] 7. Variations In the above embodiment, a liquid chromatograph has been described as an example of the chromatograph 10, but the same can be said for a gas chromatograph. In the case of a gas chromatograph, for example, a gas cylinder corresponds to the mobile phase container 28, and the gas in the gas cylinder corresponds to the mobile phase. In this case, the sample components separated in the separation column 36 are gaseous.

[0099] Furthermore, the specific configurations and the like given in the above-mentioned embodiments are merely examples and can be changed as appropriate according to the actual product. Also, the order in which the steps in the flow charts shown in the above-mentioned embodiments are processed can be changed as appropriate as long as the same results are obtained.

[0100] 7. Aspects It will be appreciated by those skilled in the art that the exemplary embodiments described above are examples of the following aspects.

[0101] (Item 1) A chromatographic apparatus according to one embodiment comprises: A chromatographic apparatus in which a mobile phase is introduced into a column together with a sample, and components in the sample separated in the column are detected by a detection unit, a test processing unit that performs a plurality of test analyses in which different amounts of sample are introduced into the column in a predetermined order according to the amounts introduced; a determination processing unit that determines whether or not to cause the test processing unit to execute a next test analysis in accordance with the predetermined order based on a detection result by the detection unit during the test analysis; an introduction amount setting processing unit that sets an introduction amount for repetition based on the introduction amount of the sample in the previously performed test analysis when the determination processing unit determines that the next test analysis is not to be performed; The sample may further include a repeated introduction processing unit that repeats an introduction process of introducing the sample into the column with the repeated introduction amount a plurality of times.

[0102] According to the chromatographic device described in paragraph 1, by performing a test analysis, it is possible to appropriately set the amount of sample introduced into the column and to repeat the introduction process multiple times with that amount. In addition, since the amount of sample introduced into the column can be automatically set, the analyst does not need to consider the amount of sample introduced into the column, and it is possible to prevent differences in the time and results of considering the amount of sample introduced into the column depending on the analyst.

[0103] (Item 2) In the chromatographic apparatus according to item 1, When the judgment processing unit determines that the next test analysis should be performed during the final test analysis of the multiple test analyses, instead of the test processing unit performing the next test analysis, the introduction amount setting processing unit may set the introduction amount for the repetition based on the introduction amount of sample during the previously performed test analysis.

[0104] According to the chromatographic device described in paragraph 2, when it is determined during the final test analysis of multiple test analyses that the next test analysis should be performed, the amount of sample introduced into the column can be set to an upper limit value, and the introduction process can be repeated multiple times at that amount.

[0105] (Item 3) In the chromatographic apparatus according to item 1 or 2, If, during the first test analysis of the multiple test analyses, the judgment processing unit determines that the next test analysis should not be performed, the introduction amount setting processing unit does not need to set the introduction amount for the repetition.

[0106] According to the chromatographic device described in paragraph 3, when it is determined during the first test analysis of multiple test analyses that the next test analysis should not be performed, the amount of sample to be introduced into the column is not set and the introduction process can be interrupted.

[0107] (Item 4) In the chromatographic apparatus according to any one of items 1 to 3, The test processing unit may perform the multiple test analyses in ascending order of the introduction amounts.

[0108] According to the chromatographic device described in paragraph 4, multiple test analyses are performed in ascending order of the amount of sample introduced, so that the amount of sample introduced into the column in one introduction process can be set to be as large as possible. Therefore, in the case of a configuration in which components in a sample are separated, the separation can be performed efficiently.

[0109] (Item 5) In the chromatographic apparatus according to item 4, The determination processing section may determine whether or not to perform a next test analysis based on a degree of separation of peaks in a detection result by the detection section during a test analysis.

[0110] According to the chromatographic apparatus described in paragraph 5, it is possible to appropriately determine whether or not to perform a next test analysis based on the degree of peak separation, which deteriorates as the amount of sample introduced into the column increases during the test analysis.

[0111] (Item 6) In the chromatographic apparatus according to any one of items 1 to 3, The test processing unit may perform the multiple test analyses in descending order of the introduction amounts.

[0112] According to the chromatographic device described in paragraph 6, since multiple test analyses are performed in descending order of the amount of sample introduced, it is possible to set the amount of sample introduced into the column in each introduction process to be as small as possible. Therefore, in the case of a configuration for performing a highly sensitive analysis to detect components contained in a small amount of sample, it is possible to minimize the amount of sample used.

[0113] (Item 7) In the chromatographic apparatus according to item 6, The determination processing section may determine whether or not to perform a next test analysis based on the intensity of a peak in a detection result by the detection section during a test analysis.

[0114] According to the chromatographic apparatus described in paragraph 7, it is possible to appropriately determine whether or not to perform a next test analysis based on the peak intensity, which decreases as the amount of sample introduced into the column during the test analysis decreases.

[0115] (Item 8) The chromatographic apparatus according to any one of items 1 to 7, Further comprising a number setting processing unit that sets the number of times of the introduction process based on the repetition introduction amount set by the introduction amount setting processing unit; The repeated introduction processing unit may perform the introduction process a number of times set by the number setting processing unit.

[0116] According to the chromatographic device described in item 8, the number of times the introduction process is performed can be appropriately set based on the repeated introduction amount set in the introduction amount setting processing unit, and the introduction process can be repeated multiple times at that number of times.

[0117] (Item 9) A method for setting a sample introduction amount according to one embodiment includes the steps of: A method for setting a sample introduction amount in a chromatographic apparatus in which a mobile phase is introduced into a column together with a sample, and components in the sample separated in the column are detected by a detection unit, comprising: a test step of performing a plurality of test analyses in which different amounts of sample are introduced into the column in a predetermined order according to the amounts introduced; a determination step of determining whether or not to execute a next test analysis in the test step according to the predetermined order based on a detection result by the detection unit during the test analysis; If the judgment step determines that the next test analysis will not be performed, the method may further include an introduction amount setting step of setting an introduction amount for repeating the introduction process of introducing a sample into the column in the chromatographic device multiple times, based on the introduction amount of the sample during the previously performed test analysis.

[0118] According to the sample introduction amount setting method described in paragraph 9, by performing a test analysis, the amount of sample to be introduced into the column can be appropriately set, and the introduction process can be repeated multiple times with that amount. In addition, since the amount of sample to be introduced into the column can be automatically set, the analyst does not need to consider the amount of sample to be introduced into the column, and it is possible to prevent differences in the time and results of considering the amount of sample to be introduced into the column from differing depending on the analyst. [Explanation of symbols]

[0119] 10 Chromatography equipment 36 Separation Column 38 Detection section 102 Test processing section 104 Judgment processing unit 106 Setting processing section 108 Repeated introduction processing section 116 Introduction amount setting processing unit 118 Number of times setting processing unit

Claims

1. A chromatographic apparatus that introduces a mobile phase into a column together with a sample, and detects components in the sample separated in the column with a detection unit, a test processing unit that performs a plurality of test analyses in which different amounts of sample are introduced into the column in a predetermined order according to the amounts introduced; a determination processing unit that determines whether or not to execute a next test analysis in the test processing unit according to the predetermined order based on a detection result by the detection unit during the test analysis; an introduction amount setting processing unit that sets an introduction amount for repetition based on the introduction amount of the sample in the previously performed test analysis when the determination processing unit determines that the next test analysis is not to be performed; a repeat introduction processing unit that repeats an introduction process of introducing the sample into the column with the repeated introduction amount a plurality of times, When the test processing unit performs the multiple test analyses in ascending order of the introduction amounts, the determination processing unit determines whether or not to perform a next test analysis based on the degree of separation of peaks in the detection result by the detection unit during the test analysis, When the test processing unit performs the multiple test analyses in descending order of the introduction amount, the judgment processing unit determines whether to perform a next test analysis based on the intensity of the peak in the detection result by the detection unit during the test analysis, a chromatographic device.

2. 2. The chromatographic apparatus of claim 1, wherein when the judgment processing unit determines that the next test analysis should be performed during the final test analysis of the multiple test analyses, instead of performing the next test analysis in the test processing unit, the introduction amount setting processing unit sets the amount of sample introduced for the repetition based on the amount of sample introduced during the previously performed test analysis.

3. 3. The chromatographic apparatus of claim 1, wherein when the judgment processing unit determines during the first test analysis of the multiple test analyses that the next test analysis will not be performed, the introduction amount setting processing unit does not set the introduction amount for the repetition.

4. Further comprising a number setting processing unit that sets the number of times of the introduction process based on the repetition introduction amount set by the introduction amount setting processing unit; The chromatographic apparatus according to claim 1 , wherein the repeated introduction processing unit performs the introduction process a number of times set by the number setting processing unit.

5. A method for setting a sample introduction amount in a chromatographic apparatus in which a mobile phase is introduced into a column together with a sample, and components in the sample separated in the column are detected by a detection unit, comprising: a test step of performing a plurality of test analyses in which different amounts of sample are introduced into the column in a predetermined order according to the amounts introduced; a determination step of determining whether or not to execute a next test analysis in the test step according to the predetermined order based on a detection result by the detection unit during the test analysis; and an introduction amount setting step for setting an introduction amount for repeating an introduction process of introducing a sample into the column in the chromatographic device a plurality of times based on the introduction amount of the sample in the previously performed test analysis when it is determined in the determination step that a next test analysis is not to be performed, When the test step is to perform the multiple test analyses in ascending order of the introduction amount, the determination step is to determine whether or not to perform a next test analysis based on a degree of separation of peaks in the detection result by the detection unit during the test analysis; A sample introduction amount setting method, in which, when the multiple test analyses are performed in descending order of the introduction amounts in the test step, it is determined in the judgment step whether or not to perform a next test analysis based on the peak intensity in the detection result by the detection unit during the test analysis.

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