JP-2026075326-A - Preparative liquid chromatography

JP2026075326AJP 2026075326 AJP2026075326 AJP 2026075326AJP-2026075326-A

Abstract

[Problem] To enable the recovery of N+1 or more sample components in a preparative liquid chromatograph equipped with N trap columns. [Solution] A preparative liquid chromatograph comprising: a separation column; a detector for detecting sample components in the eluate from the separation column; a component capture unit for introducing the eluate into one of a plurality of trap columns to capture the components; a recovery unit for collecting the eluate into a container; a flow path switching unit for switching the flow path to introduce the eluate into either the component capture unit or the recovery unit; and a control unit that controls the flow path switching unit to introduce the eluate into the component capture unit until the number of components sequentially detected with each sample introduction into the separation column is equal to the number of trap columns, and then introduce the eluate into the recovery unit after the number of components exceeds the number of trap columns. [Selection Diagram] Figure 1

Inventors

大友伊織

Assignees

株式会社島津製作所

Dates

Publication Date: 20260508
Application Date: 20241022

Claims (5)

A separation column for separating components in a sample, A detector for detecting the component in the eluate from the separation column, A chromatogram creation unit that creates a chromatogram in real time based on the detection signal obtained by the detector, A peak counting unit that sequentially counts the peaks appearing on the chromatogram, A component capture unit having multiple trap columns, which selectively introduces the eluate into one of the multiple trap columns to capture the component, A recovery unit for collecting the eluate into a predetermined container, A flow path switching unit that switches the flow path so that the eluate from the separation column is introduced into either the component capture unit or the recovery unit, A column number storage unit that stores the number of the plurality of trap columns provided in the component capture unit, A determination unit that determines whether the number of peaks sequentially counted by the peak counting unit in conjunction with a single sample introduction into the separation column exceeds the number of the multiple trap columns, A control unit controls the flow path switching unit to introduce at least the portion of the eluate containing the component detected by the detector into the component capture unit until the determination unit determines that the number of peaks exceeds the number of trap columns, and after the determination unit determines that the number of peaks exceeds the number of trap columns, to introduce at least the portion of the eluate containing the component detected by the detector into the recovery unit. A preparative liquid chromatograph having a preparative liquid chromatograph.
The collection unit holds a plurality of the containers, After the flow path is switched by the flow path switching unit to introduce the eluate into the recovery unit, the control unit controls the recovery unit to collect the portion of the eluate corresponding to each of the components detected by the detector into one of the multiple containers. The preparative liquid chromatograph according to claim 1.
The collection unit holds a plurality of the containers, After the flow path is switched by the flow path switching unit to introduce the eluate into the recovery unit, the control unit controls the recovery unit to individually recover portions of the eluate corresponding to each of the components detected by the detector into each of the multiple containers. The preparative liquid chromatograph according to claim 1.
The recovery unit further includes an injection mechanism for injecting liquid into the flow path leading to the separation column, A recovery unit control unit controls the recovery unit to inject the eluate recovered in the predetermined container into the flow path leading to the separation column. A preparative liquid chromatograph according to any one of claims 1 to 3, further comprising the above.
Furthermore, A mobile phase supply unit that supplies the mobile phase to the flow path leading to the separation column, A mobile phase supply control unit controls the mobile phase supply unit so that the mobile phase conditions when the eluate collected in the predetermined container is injected into the flow path leading to the separation column and separated by the separation column are different from the mobile phase conditions when the eluate was collected. A preparative liquid chromatograph according to claim 4, having the following features.

Description

This invention relates to a preparative liquid chromatograph. A preparative liquid chromatograph is known that uses liquid chromatography to fractionate and collect one or more components (compounds) contained in a liquid sample. In a preparative liquid chromatograph, the sample is passed through a separation column along with a mobile phase, separating the various components of the sample over time. The separated sample components are detected by a detector, such as a spectrophotometer, located downstream of the separation column, and a chromatogram is created based on the detection signal. Peaks appearing on the chromatogram are then detected from the waveform, and by opening and closing a solenoid valve in a fraction collector located downstream of the detector in accordance with the start and end of these peaks, each sample component is separated and collected into different containers. Some preparative liquid chromatographs have a function to concentrate the sample components separated in the separation column by trapping them in different trap columns (see, for example, Patent Document 1). The sample components trapped in each trap column are then eluted by flowing a predetermined solvent through the trap column and recovered in a fraction collector. By using a solvent with high elution ability, the sample components collected in the trap columns can be eluted in a short time (i.e., with a small amount of solvent), allowing for the acquisition of a solution containing high concentrations of the sample components. Furthermore, by using a highly volatile organic solvent, the subsequent step of evaporating the solvent to obtain the sample components in a solid state (drying step) can be performed in a short time. Japanese Patent Publication No. 2003-149217 A diagram showing a schematic configuration of a preparative liquid chromatograph according to one embodiment of the present invention.A block diagram showing the main components of the control/processing unit in the same embodiment.A portion of the flowchart illustrating the operation of the preparative liquid chromatograph.The continuation of the flowchart in Figure 3.A diagram showing the liquid flow before sample introduction in the same embodiment.This diagram shows the flow of liquid when the sample components are captured in the trap column in the same embodiment.This diagram shows the liquid flow when directly recovering the sample components in the same embodiment.This figure shows the flow of liquid when eluting sample components from the trap column in the same embodiment.A diagram showing a schematic configuration of a preparative liquid chromatograph according to another embodiment of the present invention.A diagram showing a schematic configuration of a preparative liquid chromatograph according to yet another embodiment of the present invention. The embodiments for carrying out the present invention will be described below with reference to the drawings. Figure 1 is a schematic diagram of the preparative liquid chromatograph according to this embodiment. This preparative liquid chromatograph comprises an LC unit 100, a component capture unit 200, an eluent supply unit 300, a fraction collector 400 (corresponding to the recovery unit in this invention), a flow path switching unit 500, and a control/processing unit 600. The LC unit 100 comprises a mobile phase container 101, a mobile phase flow path 102, and, respectively, a mobile phase supply pump 103 (corresponding to the mobile phase supply unit in this invention), an automatic sample injection device 104, a separation column 105, and a detector 106, all of which are provided on the mobile phase flow path 102. As the detector 106, various detectors used in liquid chromatography, such as an absorbance detector or a differential refractive index detector, can be used. The component capture unit 200 comprises a plurality of trap column channels 211 to 215, each of which is provided with a trap column 210; a drain channel 220, which is a channel without a trap column 210; a first column switching valve 201; and a second column switching valve 202. Each trap column 210 is filled with a collection agent for capturing sample components. The first column switching valve 201 and the second column switching valve 202 each have one common port and a plurality of selectable ports, and one of the plurality of selectable ports can be selectively connected to the common port. The plurality of trap column channels 211 to 215 and the drain channel 220 are arranged in parallel with each other, and one end of each channel 211 to 215 and 220 is connected to each of the plurality of selectable ports of the first column switching valve 201, and the other end of each channel 211 to 215 and 220 is connected to each of the plurality of selectable ports of the second column switching valve 202. The first column switching valve 201 and the second column switching valve 202 are synchronized. When one valve select