Chromatograph device

JP2025014813A5Pending Publication Date: 2026-05-13SHIMADZU SEISAKUSHO LTD
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Patent Information

Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
SHIMADZU SEISAKUSHO LTD
Filing Date
2023-07-19
Publication Date
2026-05-13

AI Technical Summary

Technical Problem

Conventional chromatograph devices require users to manually check distribution results and set detailed analysis conditions, making the process cumbersome and inefficient.

Method used

A chromatograph device with a distribution analysis condition setting unit and an analysis execution unit that automatically sets and executes distribution and analysis conditions based on predefined settings, reducing the need for manual intervention.

Benefits of technology

The device streamlines the process by allowing users to set conditions once and automatically execute distribution and analysis, minimizing the effort required for checking distribution results and analyzing components.

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Abstract

To fraction a target component in a sample by using a chromatograph device and reduce the time and effort when analyzing the fractioned target component.SOLUTION: A chromatograph device 1 includes: a fraction device 17 in which a sample container 172 storing a sample containing a target component and a fraction container 173 storing the fractioned target component are arranged; a fraction and analysis condition setting unit 42 which makes a user set a fraction condition of the target component and an analysis condition of the target component after fraction; a fraction execution unit 43 which extracts the sample from the sample container and fractions the target component contained in the sample into the fraction container according to the fraction condition after the fraction condition and analysis condition are set by the fraction and analysis condition setting unit; and an analysis execution unit 44 which extracts the target component from the fraction container following the fraction of the target component by the fraction execution unit and analyzes the target component according to the analysis condition.SELECTED DRAWING: Figure 1
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Description

[Technical field]

[0001] The present invention relates to a chromatographic device. [Background technology]

[0002] One type of liquid chromatograph is a preparative liquid chromatograph (see, for example, Patent Document 1). In a preparative liquid chromatograph, a liquid sample is introduced into a column of the liquid chromatograph, a target component contained in the liquid sample is separated from other components in the column, and only the target sample is separated into a separation container. When separating a target component from a sample, the liquid sample is often injected into a mobile phase with a high flow rate and introduced into a short column to separate the target component in a short time.

[0003] Preparative liquid chromatographs are used, for example, to separate a target component having medicinal properties in the development of new drugs in the field of drug discovery. When confirming the medicinal properties of the target component, detailed analysis is performed to confirm that there is no error in the separated target component and that the separated target component is not contaminated with impurities. In such cases, the target component is separated into a separation container, and then detailed analysis conditions for the target component are set to analyze the target component. In the detailed analysis of the target component, analysis conditions are set that increase the degree of separation between components over a longer period of time than when the target component was separated, such as by lowering the flow rate of the mobile phase or using a longer column than when the target component was separated. [Prior art documents] [Patent documents]

[0004] [Patent Document 1] International Publication No. 2018 / 163276 Summary of the Invention [Problem to be solved by the invention]

[0005] In conventional methods, after setting conditions for separating a target component in a sample and separating the target component, when analyzing it in detail, the user must check information about the separation container from which the target component was separated on the separation result screen, and then set detailed analysis conditions for the target component to analyze it, which makes separation and analysis of the target component time-consuming.

[0006] Although the case where a liquid chromatograph is used to separate and analyze a target component has been described here, the same problems as described above also occur when a chromatographic device such as a gas chromatograph is used.

[0007] The problem to be solved by the present invention is to reduce the time and effort required for separating a target component in a sample using a chromatographic device and then analyzing the separated target component. [Means for solving the problem]

[0008] The chromatographic device according to the present invention, which has been made to solve the above problems, comprises: a fractionation device in which a sample container containing a sample containing a target component and a fractionation container containing a fraction of the target component are disposed; a preparative analysis condition setting unit that allows a user to set preparative conditions for the target component and analytical conditions for the target component after separation; a preparative separation execution unit that, after the preparative separation conditions and the analytical conditions are set in the preparative separation analysis condition setting unit, collects a sample from the sample container and separates the target component contained in the sample into the preparative separation container in accordance with the preparative separation conditions; an analysis execution unit that collects the target component from the collection container and analyzes the target component according to the analysis conditions following the collection of the target component by the collection execution unit; Equipped with. Effect of the Invention

[0009] In the chromatographic apparatus according to the present invention, first, the preparative analysis condition setting unit allows a user to set preparative conditions and analysis conditions for a target component, and then the preparative separation execution unit and the analysis execution unit sequentially execute preparative separation of the target component contained in a sample and analysis of the preparative target component. Therefore, after preparative separation of the target component in a sample, the user does not need to check information about the preparative container from which the target component was preparative on the preparative result screen, thereby reducing the effort required for preparative separation and analysis of the target component. [Brief description of the drawings]

[0010] [Figure 1] 1 is a configuration diagram of a main part of a preparative liquid chromatograph system, which is one embodiment of a chromatograph device according to the present invention. [Diagram 2] 3 is a flowchart illustrating a procedure for separating and analyzing a target component contained in a sample using the preparative liquid chromatograph system of the present embodiment. [Diagram 3] 4 shows an example of a preparative analysis condition setting screen in the preparative liquid chromatograph system of the present embodiment. [Figure 4] 4 shows an example of a result display screen in the preparative liquid chromatograph system of the present embodiment. [Diagram 5] FIG. 2 is a diagram for explaining a method for determining a target for detailed analysis when a target component is fractionated into a plurality of vials in the preparative liquid chromatograph system of the present embodiment. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0011] An embodiment of a chromatographic apparatus according to the present invention will be described below with reference to the drawings. The chromatographic apparatus of this embodiment is a preparative liquid chromatographic system having a function of separating a target component contained in a sample and further performing detailed analysis of the separated target component.

[0012] 1 shows the configuration of the main components of a preparative liquid chromatograph system 1 of this embodiment. The preparative liquid chromatograph system 1 includes a preparative liquid chromatograph 10 and a control / processing unit 40.

[0013] The preparative liquid chromatograph 10 includes a mobile phase container 11, a liquid delivery pump 12, an injector 13, a preparative column 14, a first detector 15, a second detector 16, a liquid handler 17, an analytical column 24, and a third detector 25. FIG. 1 shows only one mobile phase container 11 and one liquid delivery pump 12, but the preparative liquid chromatograph 10 may include a mobile phase container 11 that contains a plurality of mobile phases individually, a liquid delivery pump 12 that delivers the mobile phases individually, and a mixer that mixes the plurality of mobile phases. The injector 13 is provided with a port for injecting a preparative sample and a port for injecting an analytical sample, and the preparative sample is introduced into the preparative column 14, and the analytical sample is introduced into the analytical column 24. The first detector 15 is a detector that nondestructively measures the components flowing out of the preparative column 14, and may be, for example, an absorptiometer. The second detector 16 is a detector that measures the components flowing out from the preparative column 14 by a method different from that of the first detector 15, and may be, for example, a mass spectrometer. The third detector 25 is a detector that measures the components flowing out from the analytical column 24, and any detector may be used.

[0014] The liquid handler 17 functions both as an injector that injects a sample into a mobile phase and as a fraction collector that fractionates a desired portion of the effluent from the fractionation column 14 and stores the fraction in a fractionation container. Inside the liquid handler 17, a plate (sample rack) 171 on which a sample vial 172 containing a sample and a fractionation vial 173 containing a fractionated target component are placed is set. The liquid handler 17 is also provided with an injection section 18 having a needle 182 inserted into the sample vial 172 and a syringe pump 181 that collects and ejects the sample through the needle 182, and a fractionation section 19 having a nozzle 191 inserted into the fractionation vial 173. In the injection section 18, under the control of the fractionation execution section 43 or the analysis execution section 44 described below, the sample or target component stored in the specified sample vial 172 is collected and injected into the injector 13. In the fraction collection section 19, the target component contained in the sample is fractionated into a fraction collection vial 173 based on detection of the target component by the first detector 15 and / or the second detector 16. The liquid handler 17 corresponds to the fraction collection device in this invention. Moreover, the sample vial 172 corresponds to the sample container, and the fraction collection vial 173 corresponds to the fraction collection container.

[0015] The control and processing unit 40 includes a storage unit 41. In the storage unit 41, for each of a large number of known components, information on the preparative conditions for preparatively separating the component and the conditions for detailed analysis performed after the component is preparatively separated are stored in a method file. These preparative conditions and analysis conditions include, for example, the type and flow rate of the mobile phase, the type of the preparative column 14 and the analytical column 24, information on the detection signal (reference detection signal) of the component in the first detector 15 (for example, absorption wavelength and absorbance when the first detector 15 is an absorption detector), information on the detection signal (reference detection signal) of the component in the second detector 16 (for example, mass-to-charge ratio and intensity of ions when the second detector 16 is a mass spectrometer), and information on the detection signal (reference detection signal) of the component in the third detector 25. The analysis conditions are set to, for example, conditions that increase the degree of separation by lowering the flow rate of the mobile phase compared to when the target component was preparatively separated or by using an analytical column 24 that is longer than the preparative column 14.

[0016] The control / processing unit 40 comprises, as functional blocks, a preparative analysis condition setting unit 42, a preparative analysis execution unit 43, an analysis execution unit 44, a judgment unit 45, and a result display unit 46. The actual entity of the control / processing unit 40 is, for example, a general personal computer, and these functional blocks are embodied by executing a dedicated preparative analysis program preinstalled in the processor. In addition, an input unit 51 consisting of a keyboard, mouse, etc., and a display unit 52 consisting of a liquid crystal display, etc. are connected to the control / processing unit 40.

[0017] Next, a procedure for preparatively separating and analyzing a target component contained in a sample using the preparative liquid chromatograph system 1 of this embodiment will be described with reference to the flowchart of FIG.

[0018] First, the user places a sample vial 172 containing a sample including a target component and a fractionation vial 173 for containing the fractionated target component on a plate 171, and sets the plate 171 in the liquid handler 17 (step 1). Then, information on the sample vial 172 and the fractionation vial 173 is registered. When multiple plates 171 are set in the liquid handler 17, the numbers of the plates 171 are also registered. In this embodiment, one plate 171 having 24 holes (vial placement parts, numbers 1 to 24) is used, and three sample vials 172 containing three samples each and 21 empty fractionation vials 173 are placed on the plate 171 and set in the liquid handler 17. Here, the sample vials 172 containing samples are placed at numbers 1 to 3, and the empty fractionation vials 173 are placed at numbers 4 to 24. The sample vials 172 and the aliquot vials 173 may be provided on different plates.

[0019] When the user instructs setting preparative analysis conditions, preparative analysis condition setting section 42 displays on display section 52 a screen for setting preparative analysis conditions for the target component contained in the sample and conditions for detailed analysis of the target component after separation.

[0020] FIG. 3 is an example of a setting screen for preparative separation conditions and analytical conditions. In this preparative separation and analysis condition setting screen 70, a vial display area 71, a preparative separation and analysis condition display area 72, a cancel button 73, and a decision button 74 are displayed. In the preparative separation and analysis condition display area 72, a plate No. field 721, a vial No. field 722, a method field 723, a name field 724, an injection amount field 725, an automatic reinjection field 726, a reinjection method field 727, and a reinjection amount field 728 are provided. In this manner, in this embodiment, the plate No. field 721, the vial No. field 722, the method field 723, the name field 724, the injection amount field 725, the automatic reinjection field 726, the reinjection method field 727, and the reinjection amount field 728 are configured to be displayed on the same screen, and the preparative separation conditions and analytical conditions can be set on the same screen. This improves the convenience for the user.

[0021] In the vial display area 71, a top view of the plate 171 set in the liquid handler 17 is displayed. In this example, only one plate 171 is set, but if multiple plates 171 are set in the liquid handler 17, the multiple plates 171 can be switched or arranged for display. In the vial display area 71, sample vials 172 containing samples and empty fraction vials 173 are displayed in a distinguishable manner based on information previously registered by the user. In the example of FIG. 3, among the vials contained in the 24-hole plate 171, the sample vials 172 numbered 1 to 3 are hatched to indicate that they contain samples. Although hatching is used here, the sample vials 172 containing samples and the empty fraction vials 173 may be made distinguishable by other display forms such as color display.

[0022] The user selects, by using the mouse or the like, from among the hatched sample vials 172 (containing samples) displayed in the vial display area 71, one containing a sample from which a target component is to be fractionated (step 2). When the user performs an operation to select a sample vial 172 in the vial display area 71, the number of the plate 171 on which the sample vial 172 is placed and the number (position) of the vial on the plate 171 are automatically entered into the plate number column 721 and the vial number column 722, respectively, in the fractionation analysis condition display area 72.

[0023] Next, the user reads out from the storage unit 41 a method file describing the separation conditions for separating a target component from the sample contained in the selected sample vial 172. When the user reads out the method file, the file name is displayed in the method column 723 of the separation analysis condition display area 72 (step 3). In addition, the name of the target component to be separated by executing the method file is read into the name column 724 of the separation analysis condition display area 72. When multiple target components are separated by one method, the names of the multiple target components are displayed in the name column 724. The user further inputs the injection amount of the sample into the injection amount column 725. Here, the user inputs the injection amount, but the injection amount may also be preset as a separation condition to be described in the method file, and the value may be automatically read and entered into the injection amount column 725.

[0024] The user then selects whether or not to automatically perform detailed analysis of the target component fractionated from the sample (step 4). This selection is made by clicking a check box provided in the automatic reinjection field 726 to input a check mark.

[0025] When a check mark is entered in the automatic reinjection field 726, the preparative analysis condition setting unit 42 accepts input into the reinjection method field 727. The user reads out from the storage unit 41 a method file describing the conditions for detailed analysis of the separated target component. When the user reads out the method file, the file name is displayed in the reinjection method field 727 in the preparative analysis condition display area 72. The user further inputs the injection amount for detailed analysis of the target component into the injection amount field 725. Here too, the user inputs the injection amount, but it is also possible to set the injection amount in advance as an analysis condition to be described in the method file, and have this value automatically read and entered into the injection amount field 725.

[0026] When the above input is completed for all samples for which the target component is to be fractionated and analyzed in detail, and the user presses the decision button 74, the preparative analysis condition setting unit 42 reads the sample selected by the user, the preparative analysis conditions for fractionating the target component from the sample, and the conditions for detailed analysis of the fractionated target component, and creates a file for executing them consecutively (step 5). When the user presses the cancel button 73, the preparative analysis conditions entered at that time are reset. For samples for which the automatic reinjection field 726 is not checked, the preparative analysis condition setting unit 42 creates an execution file for only fractionating the target component, and for samples for which the automatic reinjection field 726 is checked, creates an execution file for fractionating the target component and then automatically reinjecting the fractionated target component for detailed analysis.

[0027] After creating the preparative analysis execution file, when the user issues an instruction to start preparative separation and analysis of the target component by a predetermined input operation, the preparative separation execution unit 43 controls each part of the preparative liquid chromatograph 10 to collect a sample from the plate 171 and sample vial 172 that the user selected first in the preparative analysis condition display area 72. The target component contained in the sample is separated from other components while passing through the preparative column 14 and flows out. Based on the detection of the flowed-out target component by the first detector 15 and / or the second detector 16, the preparative separation unit 19 separates the target component into the preparative vial 173 (step 6).

[0028] The fraction collection unit 19 fractionates the target component into empty fraction collection vials 173 in ascending order of numbers. In this embodiment, since the sample vials 172 numbered 1 to 3 contain samples, the target component is fractionated in order starting from fraction collection vial 173 numbered 4. The amount of fraction collection into one fraction collection vial 173 is predetermined, and if the sample liquid containing the target component flows out of the fraction collection column 14 in excess of that amount, the fraction collection unit 19 switches the fraction collection vial 173 from which the target component is collected to the next fraction collection vial 173 numbered 5. When the target component is collected by the fraction collection unit 19, the fraction collection execution unit 43 stores information (plate number and vial number) of the fraction collection vial 173 from which the target component was collected in the memory unit 41 together with the sample name, the target component name, the detection signal of the first detector 15 at the time of collection, and the detection signal of the second detector 16 (step 7).

[0029] When an execution file for only separating the target component is created, only the target component contained in the sample is separated. On the other hand, when an execution file for separating the target component and then analyzing the separated target component in detail is created, the analysis execution unit 44 controls each part of the preparative liquid chromatograph 10 and performs detailed analysis of the separated target component using the analytical column 24 and the third detector 25 based on the conditions described in the execution file (step 8).

[0030] When the collection of the target component and detailed analysis (if execution of detailed analysis is set) for the first sample is completed, the collection execution unit 43 determines whether there are any unprocessed samples (step 9). If there are unprocessed samples (YES in step 9), the process returns to step 5, and collection of the target component and detailed analysis are performed for the unprocessed samples. If the processing of all samples is completed and there are no unprocessed samples (NO in step 9), the operation related to the collection of the target component and detailed analysis is terminated.

[0031] When the separation and detailed analysis of the target components are completed for all samples, the determination unit 45 determines the results of the detailed analysis for each of the target components that have been subjected to the detailed analysis. Specifically, for example, the detection signal (e.g., absorption spectrum or mass spectrum) of the third detector 25 acquired in the detailed analysis of the target component is compared with the reference detection signal (e.g., absorption spectrum or mass spectrum) of the target component stored in the storage unit 41, and determines whether the two match within a predetermined allowable range (step 10). If it is determined that the two match, the determination unit 45 determines that the separated product is the target component and that impurities are not mixed in. If it is determined that the two do not match, it further determines whether the detection signal (e.g., absorption spectrum or mass spectrum) of the third detector 25 acquired during the detailed analysis includes the detection signal (e.g., absorption spectrum or mass spectrum) of the target component stored in the storage unit 41. If the detection signal of the target component stored in memory unit 41 is included, it is determined that the fraction contains the target component and impurities, and if the detection signal of the target component is not included, it is determined that the fraction does not contain the target component. Specifically, for example, if a mass spectrum created from the detection signal of third detector 25 contains a mass peak in the standard mass spectrum and a mass peak not present in the standard mass spectrum, it is determined that the fraction contains the target component and impurities.

[0032] When the determination unit 45 has completed its determination for all target components that have been subjected to detailed analysis, the result display unit 46 displays the separation and analysis results on the screen of the display unit 52, including the detection signals acquired by the first detector 15 and the second detector 16 when the target components are separated from each sample, the detection signals acquired by the third detector 25 when the separated target components are subjected to detailed analysis, and the determination results by the determination unit 45 (step 11).

[0033] FIG. 4 shows an example of a result display screen 80 displayed by the result display unit 46. This example of the result display screen 80 is a case where target components A and B contained in a sample are separated and analyzed in detail. The result display screen 80 displays a total ion current (TICC) chromatogram 81 acquired when separating the target components A and B, a mass spectrum 82 acquired when performing detailed analysis on the fractions separated at positions corresponding to the peaks on the TICC chromatogram 81, and a judgment result 83 for each fraction. The mass spectrum 82 also displays the number of the fraction vial 173 that contains the fraction. In each mass spectrum 82, a mass peak of a mass-to-charge ratio that is determined to match a mass peak of the standard mass spectrum in the judgment by the judgment unit 45 (i.e., a mass peak of the target component) is displayed with a solid line, and a mass peak that is determined not to match (i.e., a mass peak of an impurity) is displayed with a dashed line. Then, the judgment result by the judgment unit 45 is displayed below each mass spectrum 82. By checking the separation / analysis result screen 80, the user can visually determine whether the separated product is the target component and whether the target component contains impurities.

[0034] Conventionally, when analyzing a target component in a sample in detail after setting conditions for separating the target component and separating the target component, the user must check information about the separation container from which the target component was separated on a separation result screen, and then set detailed analysis conditions for the target component and analyze the target component, which makes separation and analysis of the target component time-consuming.

[0035] In the preparative liquid chromatograph system 1 of this embodiment, first, the preparative analysis condition setting unit 42 allows the user to set the preparative conditions and analysis conditions for the target component, and then the preparative separation execution unit 43 and the analysis execution unit 44 successively execute the preparative separation of the target component contained in the sample and the analysis of the preparative target component. Therefore, after the target component in the sample is preparative, the user does not need to check information on the preparative container from which the target component was preparative on the preparative result screen, and the effort required for preparative separation and analysis of the target component can be reduced.

[0036] As described above, the amount of sample liquid to be collected in one fractional vial 173 is predetermined, and when the amount of sample liquid containing the target component exceeds this amount, the target component is collected in multiple fractional vials 173. Although detailed analysis may be performed on all of the multiple fractional vials 173 collected in this manner, since the fractions collected in these multiple fractional vials 173 are basically the same, it is more efficient to perform detailed analysis on only the target component collected in one of the fractional vials 173.

[0037] Hereinafter, a procedure for determining the fractionation vial 173 for performing detailed analysis when the sample liquid flowing out continuously in time from the fractionation column 14 is fractionated into a plurality of fractionation vials 173 will be described. As a specific example, a case where the second detector 16 is a mass spectrometer and the fractionation vial 173 for performing detailed analysis is determined based on mass spectrum data acquired by the mass spectrometer will be described with reference to Fig. 5. Fig. 5 shows a case where the sample liquid flowing out continuously in time from the fractionation column 14 is fractionated into three fractionation vials 173 (numbered 11 to 13).

[0038] The analysis execution unit 44 reads out mass spectrum data acquired by repeatedly performing MS scan measurements with the second detector 16 during the time period when the sample liquid that flows out continuously in time is fractionated into the plurality of fractionation vials 173. Then, an average mass spectrum is calculated from the plurality of mass spectrum data acquired during the time period when the target components are fractionated into each fractionation vial 173 (lower part of FIG. 5). Here, the mass spectrum is acquired by performing MS scan measurements. However, instead of this, three SIM measurements of target ions derived from target component A, target ions derived from target component B, and non-target ions may be repeatedly performed. Alternatively, when the times (retention times) at which target components A and B flow out of the fractionation column 14 are known, SIM measurements of target ions and non-target ions of target component A may be performed during the retention time of target component A, and SIM measurements of target ions and non-target ions of target component B may be performed during the retention time of target component B.

[0039] The analysis execution unit 44 then calculates the mass peak intensity at the mass-to-charge ratio of the target ion, which is a representative ion derived from the target component, and the mass peak intensity at the mass-to-charge ratio of the non-target ion, which is derived from something other than the target component and is measured with the same intensity regardless of time, for each of the three fractionation vials 173 (numbers 11 to 13). The mass-to-charge ratio value of the target ion is stored in advance in the storage unit 41 for each target component, and the mass-to-charge ratio value of the non-target ion is stored in advance for each fractionation condition. The mass-to-charge ratio of the non-target ion can be, for example, the mass-to-charge ratio of an ion generated from the mobile phase flowing into the detector regardless of time. In the example of FIG. 5, the mass-to-charge ratio of the target ion is 505, and the mass-to-charge ratio of the non-target ion is 256. The intensity of the mass peak is obtained from the area value or height of the mass peak.

[0040] The analysis execution unit 44 then calculates the ratio of the intensity of the mass peak of the target ion to the intensity of the mass peak of the non-target ion for each of the three fractionation vials 173 (numbers 11 to 13). The vial 173 with the largest ratio is then determined as a candidate for collecting the target component during detailed analysis, and detailed analysis is performed on the sample in the candidate fractionation vial 173 using the reinjection method and reinjection amount that were set before the start of fractionation. In this example, fractionation vial 173 numbered 12 is the candidate for collecting the target component during detailed analysis.

[0041] The analysis execution unit 44 also determines whether the intensity of the mass peak of the target ion related to the candidate vial exceeds a predetermined threshold. This threshold may be set in advance as one of the analysis conditions and stored in the storage unit 41. If the intensity of the mass peak of the target ion related to the candidate vial exceeds the threshold, the candidate vial is finally determined as the target from which the target component is to be collected during detailed analysis.

[0042] By determining the vial from which the target component is collected during detailed analysis as described above, it is not necessary to perform detailed analysis on each of a plurality of vials from which the same target component has been collected, and the efficiency of detailed analysis is improved. In addition, by selecting the one having the highest ratio of the intensity of the mass peak of the target ion to the intensity of the mass peak of the non-target ion, the target component can be collected from the vial from which a larger amount of the target component has been collected for detailed analysis. In addition, by subjecting only vials whose mass peak intensity of the target ion exceeds a threshold to detailed analysis, it is possible to reduce consumption of the target component that has been collected in only a small amount. For the target component that has been collected in only a small amount, detailed analysis can be performed using another method that can be performed with a small amount.

[0043] The above embodiment is an example, and can be appropriately modified in accordance with the gist of the present invention. In the above embodiment, when the same target component is collected in multiple vials, the target component is subjected to detailed analysis if the mass peak intensity of the target ion exceeds a threshold value. However, when the target component is collected in only one vial, the target ion mass peak intensity exceeding a threshold value may be set as a condition for detailed analysis. This can reduce consumption of the target component that is collected in only a small amount.

[0044] In the above embodiment, the ratio of the intensity of the mass peak of the target ion to the intensity of the mass peak of the non-target ion is calculated, and the vial with the largest ratio is determined as the candidate for collecting the target component during detailed analysis, but if there are no ions suitable as non-target ions, the vial with the largest intensity of the mass peak of the target ion may be determined as the candidate for collecting the target component during detailed analysis. Also, in the above embodiment, the mass peak appearing in the mass spectrum is used as an example, but when determining the candidate for collecting the target component during detailed analysis, a detection signal according to the type of detector may be used.

[0045] Although the above embodiment is a preparative liquid chromatograph system 1, a similar configuration to the above can also be adopted in a system equipped with a gas chromatograph instead of a liquid chromatograph.

[0046] [Aspects] It will be apparent to those skilled in the art that the above-described exemplary embodiments are illustrative of the following aspects.

[0047] (Section 1) A chromatographic apparatus according to one aspect of the present invention comprises: a fractionation device in which a sample container containing a sample containing a target component and a fractionation container containing a fraction of the target component are disposed; a preparative analysis condition setting unit that allows a user to set preparative conditions for the target component and analytical conditions for the target component after separation; a preparative separation execution unit that, after the preparative separation conditions and the analytical conditions are set in the preparative separation analysis condition setting unit, collects a sample from the sample container and separates the target component contained in the sample into the preparative separation container in accordance with the preparative separation conditions; an analysis execution unit that collects the target component from the collection container and analyzes the target component according to the analysis conditions following the collection of the target component by the collection execution unit; Equipped with.

[0048] In the chromatographic device according to paragraph 1, first, the preparative analysis condition setting unit allows a user to set preparative conditions and analytical conditions for the target component, and then the preparative execution unit and the analytical execution unit execute preparative separation of the target component contained in the sample and analysis of the preparatively separated target component in succession. Therefore, after preparative separation of the target component in the sample, the user does not need to check information on the preparative result screen about the preparative container from which the target component was separated, and this reduces the effort required for preparative separation and analysis of the target component.

[0049] (Section 2) The chromatographic apparatus according to paragraph 2 is the chromatographic apparatus according to paragraph 1, the preparative analysis condition setting unit further allows a user to set whether or not to execute analysis of the target component after the preparative analysis condition setting unit has separated the target component; When a user has set that an analysis of the target component is to be performed, the analysis execution unit performs the analysis of the target component following separation of the target component.

[0050] In the chromatographic apparatus according to paragraph 2, a user can selectively perform detailed analysis only on target components that the user considers require detailed analysis.

[0051] (Section 3) The chromatographic apparatus according to paragraph 3 is the chromatographic apparatus according to paragraph 1 or 2, The analysis execution unit executes an analysis of the target component based on whether a detection signal acquired when the target component is separated satisfies a predetermined criterion.

[0052] The predetermined criterion may be, for example, that the magnitude of the detection signal acquired during the separation of the target component exceeds a predetermined threshold. In the chromatographic device according to the third aspect, the target component is analyzed in detail only when a sufficient amount of the target component that satisfies the predetermined criterion is separated, so that consumption of the target component due to the detailed analysis can be suppressed when the amount of the target component separated is small.

[0053] (Section 4) The chromatographic apparatus according to paragraph 4 is the chromatographic apparatus according to any one of paragraphs 1 to 3, When the fractionation execution unit collects target components in multiple fractionation containers in succession over time, the analysis execution unit performs analysis only on the target component contained in any one of the multiple fractionation containers.

[0054] Since the amount that can be separated into one collection vessel is predetermined, if the amount of the target component is greater than that amount, the same target component will be separated into multiple collection vessels in succession over time. In the chromatographic device according to paragraph 4, the collection vessel from which the largest amount of the target component has been separated is selected from among the multiple collection vessels, and detailed analysis is performed only on the target component separated into that collection vessel, thereby improving the efficiency of analysis compared to performing detailed analysis on all of the same target component separated into multiple collection vessels.

[0055] (Section 5) The chromatographic apparatus according to paragraph 5 is the chromatographic apparatus according to paragraph 4, The analysis execution unit executes analysis only for the target component contained in one collection vessel that has the largest detection signal for the target component acquired while the target component is being collected into the multiple collection vessels.

[0056] In the chromatographic apparatus according to the fifth aspect, the target component is collected from the one of the plurality of fraction collection vessels from which the largest amount of the target component has been collected, and detailed analysis is performed, so that detailed analysis can be performed more accurately.

[0057] (Section 6) The chromatographic apparatus according to claim 6 is the chromatographic apparatus according to claim 5, The detection signal is the intensity of ions generated from the target component measured by a mass spectrometer, and the analysis execution unit performs analysis only on the target component contained in one separation container that has the largest measured intensity of ions generated from the target component relative to the intensity of ions generated from a predetermined component other than the target component, regardless of time of day, measured by a mass spectrometer.

[0058] The chromatographic device according to paragraph 6 uses a measurement signal obtained by a mass spectrometer that has high compound discrimination capability, and therefore can identify with high accuracy the separation vessel from which the greatest amount of the target component has been separated.

[0059] (Section 7) The chromatographic apparatus according to item 7 is the chromatographic apparatus according to any one of items 1 to 6, The separation conditions and the analysis conditions can be set on the same screen.

[0060] In the chromatographic device of item 7, the separation conditions and analysis conditions can be set on the same screen, improving user convenience. [Explanation of symbols]

[0061] 1. Preparative liquid chromatography system 10. Preparative Liquid Chromatography 11...Mobile phase container 12...Liquid delivery pump 13...Injector 14…Preparative column 15…First detector 16…Second detector 17…Liquid Handler 171…Plate 172... Vial containing sample 173... Vial containing target component 18...Injection part 181...Syringe pump 182...Needle 19...Preparative section 191…Nozzle 24…Analytical column 25…Third detector 40...Control and processing section 41...Storage section 42…Preparative analysis condition setting section 43… Fractionation Execution Department 44…Analysis Execution Department 45…Judgment section 46...Result display area 51...Input section 52...Display section 70…Preparative analysis condition setting screen 71…Vial display area 72…Preparative analysis conditions display area 721…Plate number column 722…Vial No. column 723...Method column 724…Name field 725…Injection amount field 726…Automatic refill field 727…Reinjection method column 728…Reinjection amount column 73...Cancel button 74...Confirmation button 80…Preparation / analysis results screen 81…Total ion current chromatogram 82...Mass spectrum 83…Judgment result

Claims

1. a fractionation device in which a sample container containing a sample containing a target component and a fractionation container containing a fraction of the target component are disposed; a preparative analysis condition setting unit that allows a user to set preparative conditions for the target component and analytical conditions for the target component after separation; a preparative separation execution unit that, after the preparative separation conditions and the analytical conditions are set in the preparative separation analysis condition setting unit, collects a sample from the sample container and separates the target component contained in the sample into the preparative separation container in accordance with the preparative separation conditions; an analysis execution unit that collects the target component from the collection container and analyzes the target component according to the analysis conditions following the collection of the target component by the collection execution unit; A chromatographic apparatus comprising:

2. the preparative analysis condition setting unit further allows a user to set whether or not to execute analysis of the target component after the preparative analysis condition setting unit has separated the target component; The chromatographic apparatus according to claim 1 , wherein the analysis execution unit executes the analysis of the target component following separation of the target component when execution of the analysis of the target component is set by a user.

3. The chromatographic apparatus according to claim 1 , wherein the analysis execution unit executes the analysis of the target component based on whether a detection signal acquired when the target component is separated satisfies a predetermined criterion.

4. 2. The chromatographic apparatus according to claim 1, wherein, when the fraction collection unit collects target components in a plurality of fraction collection containers in succession in time, the analysis execution unit performs analysis on only the target component contained in any one of the plurality of fraction collection containers.

5. 5. The chromatographic apparatus according to claim 4, wherein the analysis execution unit performs analysis only on the target component contained in one collection vessel having the largest detection signal of the target component acquired while the target component is being collected into the plurality of collection vessels.

6. 6. The chromatographic apparatus according to claim 5, wherein the detection signal is an intensity of ions generated from the target component measured by a mass spectrometer, and the analysis execution unit performs analysis only for the target component contained in one fractionation container in which the measured intensity of ions generated from the target component is the largest relative to a predetermined intensity of ions generated from other than the target component, measured by the mass spectrometer, regardless of time of day.

7. 2. The chromatographic apparatus according to claim 1, wherein the separation conditions and the analysis conditions can be set on the same screen.