JP2536327B2 - Liquid chromatograph fractionator - Google Patents

Description

Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for collecting sample components using a liquid chromatograph. When a sample component is separated by a liquid chromatograph and an intended component is collected, an electromagnetic three-way valve is inserted into a pipe line connected to a column outlet, and this three-way valve is used. Normally, the column effluent is allowed to flow to the drainage reservoir by opening it to the drainage reservoir side, and the three-way valve is opened to the preparative container side according to the time when the target component comes out to prevent the target component from flowing out. After that, I switched the three-way valve to the drainage reservoir side. This may be sufficient if there is only one component to be extracted and collected in the sample, but in the case of collecting and collecting multiple types of components, the three-way valve is switched to the drain side after the outflow of one component, The separated component remains in the separated component outflow passage, and when the next component begins to flow out from the column and the three-way valve is switched to the container side again, it remains in the separated component outflow passage. The former preparative component flows into the container for the new preparative component, and is mixed as an impurity in the subsequent new target component. In this case, the residual liquid amount is about 50 microliters, but in the conventional automatic preparative device using the solenoid valve, it was used after being aware that the preparative component was contaminated with the preparatory fraction. . SUMMARY OF THE INVENTION It is an object of the present invention to prevent the above-mentioned preparative component from being contaminated by a component that has flowed out before, which occurs when a sample component is separated and collected by a liquid chromatograph. . According to the operation schedule of the three-way valve, the three-way valve is opened to the side of the preparative container by starting the outflow of the target component from the column, and a predetermined time elapses after the outflow of the target component. Therefore, the three-way valve was opened to the drain side. The column effluent of a liquid chromatograph is usually a mobile phase liquid, and a mobile phase solution containing a sample component while the sample component is flowing out, that is, while a chromatographic peak appears. Has become. Therefore, if the three-way valve is opened to the side of the preparative container for a certain period of time after the end of the peak of one target component, only the mobile phase of the chromatograph will flow in the flow path from the three-way valve to the preparative container, and Since the flow path to the preparative container is washed with this pure mobile phase, there is no risk of contamination during the preparative separation of the next component. FIG. 1 shows the main part of the apparatus. 1 is a liquid chromatograph column, 2 is a liquid flow path connected to this column, 3 is an electromagnetic three-way valve inserted in this flow path, 2
1 is a drainage flow path, 22 is a preparative flow path, 4 is a drainage reservoir, and 5 is a preparative container exchange table for preparative components, which is held by a preparative container 6. 7 is a container exchange table drive mechanism, and 8
Controls the switching of the solenoid valve 3 and the rotation of the exchange table drive mechanism 7 by the control device. Reference numeral 9 is a chromatographic detector inserted in the flow path 2. The controller 8 is instructed to sort out the number and the number of peak components of the chromatogram of the fluid flowing out from the liquid chromatograph, and when the rising edge of the peak is detected by the output signal of the detector 9. , It is determined which peak from the sample introduction, and if it is the designated preparative component, the electromagnetic three-way valve 3 is opened to the preparative flow path 22 and three-way for a predetermined time after the end of the peak. After maintaining the state of the valve 3 as it is, the three-way valve 3 is opened to the drainage flow path 21, the exchange table drive device 7 is controlled, and the preparative container 6 corresponding to the next preparative component is collected. Moved below the flow path 22,
Be prepared for the next rising peak of the preparative component. FIG. 2 shows a chromatogram. In this chromatogram, A and B are peaks of preparative components. The control device 8 detects the rising of the peak A, opens the solenoid valve 3 to the side of the preparative flow path, and switches the three-way valve 3 to the side of the preparative flow path for a certain purge period P even after the end of the component A. Then, switch to the drainage flow passage 21 side. S indicates a period in which the three-way valve is opened to the separation flow passage side, and L indicates a period to open the drainage flow passage side. During the purging period P, the liquid phase fluid of the chromatograph is collected in the separation channel 22.
Since it flows through the preparative component, the preparative component is not washed away and enters the container for the component and does not contaminate the next component. FIG. 3 is a flow chart of the sorting operation of the control device 8. As an initial operation, the electromagnetic three-way valve 3 is connected to the drainage passage 2
Open to side 1. A peak is detected (a), it is determined whether the peak is a designated peak (b), and if the determination is YES, the electromagnetic three-way valve 3 is opened (c) to the preparative flow path side, and the process returns to (a). While the peak continues, the operation is a, b, c, a
I am going around. When the peak ends, the step (a) becomes N0. When the step (a) becomes N0, it is checked whether or not the three-way valve 3 is on the preparative side (d) If the preparative side, the timing operation is started to wait for a predetermined period of time (e), and the electromagnetic three-way valve 3 is drained. The flow path 21 side is opened (f) and returned to (a). In the above-mentioned embodiment, the column outflow fluid during the washing period after the end of the peak of one preparative component is also received in the preparative container, and the preparative component is diluted. If you want to avoid dilution,
Raise one preparative container 6 on the container exchange table 5 to hold a container for receiving drainage during the washing period in between, and after completion of the peak of one preparative component, rotate the exchange table to another container. You may receive drainage during the washing period. According to the present invention, even if the sample components of a liquid chromatograph are automated using an electromagnetic three-way valve, contamination by the preceding components of the separated components can be prevented and the purity can be improved. High component collection is possible.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a perspective view of an essential part of an apparatus according to an embodiment of the present invention. FIG. 2 is an operation explanatory view of an apparatus according to the present invention. FIG. 3 is an operation of a control apparatus according to the above-described embodiment of the present invention. Flowchart [Description of symbols] 1 Column 2 Liquid flow path 3 Electromagnetic three-way valve 4 Drainage reservoir 5 Container exchange table 6 Collection container 7 Exchange table drive mechanism 8 Controller 9 Chromatographic detector 21 Drainage flow path 22 Preparative flow Road

Claims (1)

(57) [Claims] A three-way valve for switching the liquid chromatograph effluent to the drainage flow path and the separation flow path is provided on the separation flow path side during the preparative component outflow and for a predetermined time after the outflow of the preparative component. A fractionation device in a liquid chromatograph, characterized in that it is switched to the drainage flow path side during switching and other times.