Preparative chromatograph system

Abstract

To enable a user to easily recognize the purpose of each fraction collected in a collection container on the basis of preparation result information.SOLUTION: A preparative chromatograph system includes a separation column 16, a chromatograph part 2 having a detector 18, a fraction collector 4 having a collection container 24, a controller 6 configured so as to control operation of the fraction collector 4, an information processing device 8 configured so as to perform information processing about preparation operation of the fraction collector 4 and a display 10 for displaying information outputted from the information processing device 8. The information processing device 8 divides chromatograms into fraction sections that respectively correspond to all fractions collected in the collection container 24 by associating all fractions collected in the fraction collector 4 with created chromatograms, and creates preparation result information obtained by attaching respective preparation purposes of fractions corresponding to all fraction sections on the basis of a preparation condition to output the preparation result information to the display 10.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] The present invention relates to a preparative chromatography system.

Background Art

[0002] There is known a preparative chromatography system that separates a plurality of components contained in a sample from each other using a chromatograph such as high-performance liquid chromatography, and collects portions containing each component in the eluate from the separation column into individual collection containers (see Patent Document 1).

[0003] For automatic fractionation by a preparative chromatography system, there are fractionation by waveform processing, fractionation by a time program, and the like. In fractionation by waveform processing, peaks of components appearing in a chromatogram obtained by a chromatograph are detected under preset conditions, and the operation of a fraction collector is controlled so that portions detected as peaks on the chromatogram in the eluate from the separation column are sequentially collected into individual collection containers. In fractionation by a time program, the operation of a fraction collector is controlled based on a time program set so that a desired peak portion is fractionated on a chromatogram previously obtained for a sample.

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0005] In a fractionation chromatography system, after the above-described automatic fractionation is performed, fractionation result information indicating which fraction interval on the chromatogram (the interval on the chromatogram corresponding to the portion of the eluate collected in the collection container) is collected in which collection container is presented to the user. However, with the fractionation result information presented to the user by conventional systems, it has not been possible to easily grasp for what purpose each fraction interval on the chromatogram was collected in the collection container. Therefore, for example, even if a certain portion on the chromatogram was dropped into the collection container to purge the inside of the nozzle of the fraction collector, it was not easy to distinguish just by looking at the analysis result whether the fraction interval was dropped into the collection container for the purpose of purging or was collected in the collection container due to false detection as a peak.

[0006] The present invention has been made in view of the above problems, and an object thereof is to enable a user to easily recognize for what purpose each fraction interval on the chromatogram collected in the collection container was fractionated based on the fractionation result information presented after the fractionation of the sample is completed.

Means for Solving the Problems

[0007] In the fractionation chromatography system according to the present invention, a chromatography unit having a separation column for separating components contained in a sample from each other, and a detector fluid-connected downstream of the separation column and outputting a signal based on the component concentration of the eluate from the separation column; a fraction collector having a plurality of collection containers and performing a fractionation operation of dropping the eluate from the separation column from a nozzle into the collection containers for collection downstream of the chromatography unit; a controller configured to control the operation of the fraction collector based on preset fractionation conditions; an information processing device configured to perform information processing related to the fractionation operation of the fraction collector; A display for displaying information output from the information processing device, and The information processing device is configured to output, to the display, a chromatogram created based on a signal from the detector of the chromatograph unit, with collection information including a fraction section on the chromatogram collected in the collection container by the fraction collector and the collection purpose for which the fraction section was collected added thereto.

Advantages of the Invention

[0008] According to the preparative chromatography system of the present invention, since the chromatogram with the collection information including the fraction section on the chromatogram collected in the collection container by the fraction collector and the collection purpose for which the fraction section was collected added thereto is configured to be output to the display, the user can easily recognize for what purpose each fraction section on the chromatogram collected in the collection container was preparatively separated.

Brief Description of the Drawings

[0009]

Figure 1

Figure 2

Figure 3

Modes for Carrying Out the Invention

[0010] Hereinafter, with reference to the drawings

[0011] Hereinafter, an embodiment of the preparative chromatography system according to the present invention will be described.

[0012] As shown in FIG. 1, the preparative chromatography system 1 includes a chromatograph unit 2, a fraction collector 4, a controller 6, an information processing device 8, and a display 10.

[0013] The chromatograph unit 2 includes a liquid delivery pump 12, an autosampler 14, a separation column 16, and a detector 18. The liquid delivery pump 12 delivers the mobile phase toward the separation column 16. The separation column 16 is for separating a plurality of components in the sample injected into the mobile phase from each other. The autosampler 14 is a device that injects the sample into the mobile phase flowing toward the separation column 16. The detector 18 is provided downstream of the separation column 16 and outputs a signal with an intensity corresponding to the component concentration in the eluate from the separation column 16.

[0014] The fraction collector 4 includes a nozzle 20 and a three-way solenoid valve 22. The nozzle 20 can move at least in the horizontal plane direction. The nozzle 20 is fluid-connected downstream of the detector 18 of the chromatograph unit 2. Further, a plurality of collection containers 24 are arranged in the region within the movement range of the nozzle 20, and the eluate from the separation column 16 can be dropped by positioning the nozzle 20 above an arbitrary collection container 24. The three-way solenoid valve 22 is provided upstream of the nozzle 20 and is provided to switch and guide the eluate that has passed through the detector 18 to either the nozzle 22 or the drain.

[0015] The controller 6 controls the operations of the chromatograph unit 2 and the fraction collector 4 based on the fractionation conditions given from an information processing device 8 described later. The controller 6 is a device including an electronic circuit containing a CPU (central processing unit), an information storage memory, and the like.

[0016] The information processing device 8 is a computer device for performing various information processes. For the information processing device 8, fractionation conditions are set by the user so that fractions of the eluate containing a desired component in the sample are respectively collected in the collection containers 24. The fractionation conditions include the flow rate of the mobile phase, the sample injection volume, the temperature of the separation column 16, the collection conditions of the fraction collector 4, and the like. The collection conditions of the fraction collector 4 are conditions for determining the timing of dropping and collecting the eluate from the nozzle 20 into the collection container 24. When performing fractionation by waveform processing of the chromatogram, the peak detection conditions for detecting the peaks appearing in the chromatogram are included. When performing fractionation by the time program, the time program for collecting the desired component into each collection container 24 is included. Further, the collection conditions of the fraction collector 4 also include the purge time for purging the nozzle 20 after collecting the portion of the eluate corresponding to the peak portion appearing in the chromatogram.

[0017] The information processing device 8 provides the fractionation conditions set by the user to the controller 6. The controller 6 controls the operations of the chromatograph unit 2 and the fraction collector 4 based on the information regarding the fractionation conditions given from the information processing device 8, and sequentially collects the fractions of the eluate from the separation column 16 into the collection containers 24.

[0018] Furthermore, each time a portion of the eluate is collected in the collection container 24, the controller 6 transmits to the information processing device 8 collection information including, in addition to the retention time of the fraction section on the chromatogram corresponding to the portion of the eluate collected in the collection container 24, the purpose of collecting that fraction section, and the identification information of the collection container 24 in which that fraction section was collected. The purpose of collecting the fraction section is information indicating whether that fraction section is collected in the collection container 24 as a collection target portion (peak portion on the chromatogram) of the eluate from the separation column 16 or as a non-collection target portion that is not a collection target portion. The fraction section that becomes a non-collection target portion is, for example, a fraction section that was only dropped into an empty collection container 24 for purging the nozzle 20.

[0019] The information processing device 8 creates a chromatogram of the sample based on the output signal from the detector 18 read via the controller 6, and adds to the created chromatogram the fractionation intervals collected in the collection container 24 and the collection information for each fractionation interval based on the collection information received from the controller 6. In this way, the fractionation result information with the collection information for each fractionation interval collected in the collection container 24 added to the chromatogram, as shown in FIG. 2, is created by the information processing device 8.

[0020] The display 10 is a device that is communicably connected to the information processing device 8 and displays the information output from the information processing device 8. When the information processing device 8 creates the fractionation result information, it outputs the created fractionation result information to the display 10 in response to a request from the user or automatically, and presents it to the user through the display 10.

[0021] In the fractionation result information of FIG. 2, the fractionation intervals respectively collected in the collection container 24 are shown on the chromatogram. 1-1, 1-2, 1-3, 1-4, and 1-5 added to each fractionation interval are the identification information of the collection container 24 in which the fractionation interval is collected (for example, the number indicating the location where the collection container 24 is set in the fraction collector 4). It is shown that the fractionation intervals collected in the collection containers 24 of 1-1, 1-3, and 1-5 are peak portions, and the fractionation intervals collected in the collection containers 24 of 1-2 and 1-4 are the fractionation intervals that were only dropped from the nozzle 20 to the collection containers 24 of 1-2 and 1-4 for purging the nozzle 20.

[0022] As described above, by indicating not only which collection container 24 each fraction interval on the chromatogram is collected in the fractionation result information, but also the collection purpose indicating for what purpose each fraction interval is collected, it is useful for the user referring to the fractionation result information to verify whether the setting of the fractionation conditions is appropriate. For example, although noise such as a peak appears in the fraction interval with the identification information 1-2 of the collection container 24 attached, since information indicating that the collection purpose is purge is added, the user can easily determine that the noise is not misdetected as a peak and collected in the collection container 24, but is a fraction interval dropped into the collection container for the purpose of purge.

[0023] In this embodiment, the controller 6 and the information processing device 8 are provided as separate devices, but the controller 6 and the information processing device 8 can also be realized by a single computer device.

[0024] An example of the operation of this fractionation chromatograph system 1 will be described using the flowchart of FIG. 3 together with FIG. 1.

[0025] When the user sets the fractionation conditions in the information processing device 8 and instructs the start of fractionation, an instruction is transmitted from the controller 6 to the chromatograph unit 2 and the fraction collector 4, and the sample is injected into the mobile phase by the autosampler 14 (step 101). After the sample is injected into the mobile phase, when the controller 6 determines that the collection target portion (peak portion) has reached the fraction collector 4, the controller 6 controls the fraction collector 4 so that the collection target portion is collected in an empty collection container 24 (steps 102, 103). At this time, the controller 6 transmits the collection information of the portion to the information processing device 8. The information processing device 8 designates the section corresponding to the eluate portion collected in the collection container 24 among the chromatogram being created as a fraction section, and adds the collection information of the fraction section to the fraction section (step 104). Here, a notation of "peak" indicating that it has been collected as a peak portion is added to the corresponding fraction section on the chromatogram.

[0026] Thereafter, until the portion of the eluate corresponding to the next collection target part reaches the fraction collector 4, the controller 6 moves the nozzle 20 onto a new empty collection container 24, drops the eluate into the collection container 24 for a preset purge time, and purges the nozzle 20 (step 105). Also at this time, the controller 6 transmits the collection information of the portion of the eluate collected in the collection container 24 to the information processing device 8. The information processing device 8 designates the section corresponding to the portion of the collected eluate in the chromatogram being created as a fraction section, and adds the collection information of that fraction section to the fraction section (step 106). Here, the notation "purge" indicating that the fraction section has been collected in the collection container 24 for purging the nozzle 20 is added to the fraction section.

[0027] The steps of steps 102 to 106 above are repeatedly executed until the fractionation of all the collection target components in the sample is completed (or until a preset fractionation time has elapsed since the sample was injected). When the fractionation of the sample is completed (step 107), the information processing device 8 outputs the created fractionation result information to the display 10, and presents the fractionation result information to the user through the display 10. Although the collection information indicating the purpose of collecting the fraction section is displayed by "peak", "purge", etc., it may also be displayed by symbols (〇, △) indicating peak or purge, or color-coded and displayed for each collection information indicating the purpose of collecting the fraction section.

[0028] The embodiments described above are merely examples of embodiments of the fractionation chromatograph system according to the present invention, and the embodiments of the fractionation chromatograph system according to the present invention are as follows.

[0029] In one embodiment of the fractionation chromatograph system according to the present invention, a chromatograph unit having a separation column for separating components contained in a sample from each other, and a detector fluid-connected downstream of the separation column and outputting a signal based on the component concentration of the eluate from the separation column; A fraction collector having a plurality of collection containers and performing a fractionation operation of collecting the eluate from the separation column from a nozzle into the collection containers drop by drop downstream of the chromatograph unit, A controller configured to control the operation of the fraction collector based on preset fractionation conditions, An information processing device configured to perform information processing related to the fractionation operation of the fraction collector, A display for displaying information output from the information processing device, and comprising: The information processing device is configured to add a chromatogram created based on a signal from the detector of the chromatograph unit to a fractionation section on the chromatogram collected in the collection container by the fraction collector and collection information including a collection purpose for which the fractionation section was collected, and output the result to the display.

[0030] In the first aspect of the above embodiment, the controller is configured to collect, in the collection containers, a collection target portion containing a component to be collected in the eluate of the separation column and a non-collection target portion that is not the collection target portion in the eluate of the separation column, respectively. The collection information includes information for distinguishing whether each fractionation section on the chromatogram corresponds to a fractionation section of the collection target portion or a fractionation section of the non-collection target portion.

[0031] In the first aspect, the non-collection target portion may be the eluate dropped from the nozzle into the collection container for purging inside the nozzle of the fraction collector.

[0032] In the above case, the collection information may include identification information of the collection container in which each fractionation section was collected.

Explanation of Reference Numerals

[0033] 1 Fractionation Chromatography System 2 Chromatograph Unit 4 Fraction Collector 6 Controller 8 Information Processing Device 10 Display 12 Liquid Delivery Pump 14 Auto Sampler 16 Separation Column 18 Detector 20 Nozzle 22 Three-way Solenoid Valve 24 Fraction Collector

Claims

1. A chromatograph unit having a separation column for separating components contained in a sample from each other, and a detector fluid-connected downstream of the separation column for outputting a signal based on the component concentration of the eluate from the separation column; A fraction collector having a plurality of collection containers and performing a fractionation operation of dropping and collecting the eluate from the separation column from a nozzle into the collection containers downstream of the chromatograph unit; A controller configured to control the operation of the fraction collector based on preset fractionation conditions; An information processing device configured to perform information processing regarding the fractionation operation of the fraction collector; A display for displaying information output from the information processing device, comprising: The information processing device is configured to output to the display a chromatogram created based on the signal of the detector of the chromatograph unit, with additional collection information including a fractionation section on the chromatogram collected by the fraction collector into the collection container and the collection purpose for which the fractionation section was collected. A preparative chromatograph system.

2. The controller is configured to collect in the collection containers, respectively, a collection target portion containing a component to be collected in the eluate of the separation column and a non-collection target portion that is not the collection target portion in the eluate of the separation column; The collection information includes information for distinguishing whether each fractionation section on the chromatogram corresponds to a fractionation section corresponding to the collection target portion or a fractionation section corresponding to the non-collection target portion. The preparative chromatograph system according to claim 1.

3. The non-collection target portion is the eluate dropped from the nozzle into the collection container for purging inside the nozzle of the fraction collector. The preparative chromatograph system according to claim 2.

4. The collection information includes identification information of the collection container in which each fractionation section was collected. The preparative chromatograph system according to claim 2.

Images