Patent ID: 12222340

DETAILED DESCRIPTION OF THE INVENTION

Hereinafter, an embodiment of a preparative liquid chromatograph according to the present invention will be described with reference to the drawings.

As shown inFIG.1, the preparative liquid chromatograph includes a separation channel2, a liquid feeding pump4(PUM), an injector6(INJ), a separation column8(COL), a detector10(DET), a fraction collector12(FRA), and a controller14.

The liquid feeding pump4feeds a mobile phase in the separation channel2. The injector6is a device that injects a sample into the mobile phase flowing through the separation channel2. The separation column8is provided downstream of the injector6on the separation channel2, and the components of the sample injected into the mobile phase by the injector6are separated from each other in the separation column8. The detector10is provided downstream of the separation column8on the separation channel2, and a peak of each component separated in the separation column8is detected based on a detection signal of the detector10.

The fraction collector12is a device for fractionating and collecting an eluate from the separation column8into a plurality of containers at a downstream of the detector10. The fraction collector12includes a movable probe16and a switching valve18for switching and guiding the channel on the outlet side of the detector10to the probe16side and to the drain side. In addition, the fraction collector12is provided with a plurality of peak collection containers20for collecting a portion including peaks of collection target components (peak portion) in the eluate from the separation column8, and a plurality of waste liquid collection containers22for collecting a waste liquid portion not including a collection target peak.

The operation of the fraction collector12is controlled by the controller14. The controller14can be realized by a computer device for performing operation management of the preparative liquid chromatograph. The controller14is configured to detect a collection target peak from a chromatogram obtained from the detection signal of the detector10according to an extraction condition set in advance by a user, and fractionate and collect a peak portion including the collection target peak in individual peak collection containers20. Furthermore, the controller14is configured to collect at least a part of the waste liquid portion not including the collection target peak in the waste liquid collection container22in order to prevent loss of the collection target components.

The user can designate at least one collection target peak to be collected in the peak collection container20with reference to, for example, a chromatogram acquired in advance for the sample displayed on a display communicable with the controller14. The controller14controls the fraction collector12based on the detection signal of the detector10so as to collect the peak portion including the collection target peak designated by the user in the individual peak collection containers.

There is a high possibility that the collection target components that have not been collected in the peak collection container20are included in waste liquid portions before and after the peak portion. Therefore, the controller14may be configured to set, when the collection target peak is designated by the user, the waste liquid portions before and after the designated collection target peak as the waste liquid portion to be collected in the waste liquid collection container22. In this case, the user may optionally designate how much the waste liquid portions before and after the collection target peak are collected in the waste liquid collection container22.

An example of an operation of separating and extracting a sample in this embodiment will be described with reference toFIG.1and the flowchart ofFIG.2.

When a sample is injected into a mobile phase flowing through the separation channel2by the injector6, components in the sample are temporally separated in the separation column8, and the separated components are introduced into the detector10, whereby a detection signal based on the concentration of each component is acquired. The controller14detects elution of the collection target peak designated in advance by the user from the separation column8based on the detection signal of the detector10(step101). For detection of a peak, for example, a method of detecting a start point and an end point of a peak by comparing a slope in a chromatogram with a preset threshold value can be used.

At the beginning when sample separation and extraction are started, the switching valve18of the fraction collector12connects the channel on the outlet side of the detector10to the drain side. When detecting the elution of the collection target peak from the separation column8, the controller14switches the switching valve18so that the channel on the outlet side of the detector10is connected to the probe16at the timing when a predetermined amount of the waste liquid portion before the collection target peak reaches the switching valve18(step102). As a result, the eluate from the separation column8is dropped from the tip of the probe16. The controller14causes the fraction collector12to collect a predetermined amount of the waste liquid portion before the collection target peak in the waste liquid collection container22(step103), then collect the peak portion including the collection target peak in the peak collection container20(step104), and further collect a predetermined amount of the waste liquid portion after the collection target peak in the waste liquid collection container22(step105). The waste liquid portion before the collection target peak and the waste liquid portion after the collection target peak are collected in waste liquid collection containers22different from each other.

After the waste liquid portion after the collection target peak is collected in the waste liquid collection container22, the controller14switches the switching valve18so as to connect the outlet of the detector10to the drain side (step106). Thereafter, when the next collection target peak is present, the process returns to the step101and waits until the next collection target peak is eluted from the separation column8, and the steps102to106are repeated.

In the above operation, only the waste liquid portions before and after the collection target peak in the eluate from the separation column8are collected in the waste liquid collection container22, but the present invention is not limited thereto, and all of the waste liquid portion from the start to the end of the separation and extraction of the sample may be collected in the waste liquid collection container22. An example of an operation of collecting all of the waste liquid portion from the start to the end of the separation and extraction of a sample in the waste liquid collection container22will be described with reference toFIG.1and the flowchart ofFIG.3.

When a sample is injected into a mobile phase flowing through the separation channel2by the injector6, at this time point, the controller14switches the switching valve18of the fraction collector12to a state in which the channel on the outlet side of the detector10is connected to the probe16side (step201), and causes the fraction collector12to collect the waste liquid portion in the waste liquid collection container22(step202). When detecting that the collection target peak is eluted from the separation column8(step203), the controller14moves the probe16to a position on an empty peak collection container20at the timing when the peak portion reaches the switching valve18, and collects the peak portion in the peak collection container20(step204).

When the collection of the peak portion in the peak collection container20is completed, the probe6is moved onto the waste liquid collection container22again to collect the waste liquid portion in the waste liquid collection container22(step205). Thereafter, the controller14repeatedly executes the steps202to205until the separation and extraction of the sample are completed, and when the separation and extraction of the sample are completed, the switching valve18is switched to the drain side (step207). A plurality of waste liquid collection containers22can be used to collect the waste liquid portion.

The embodiment described above is merely an example of an embodiment of a preparative liquid chromatograph according to the present invention. The embodiment of a preparative liquid chromatograph according to the present invention is as follows.

A first embodiment of the preparative liquid chromatograph according to the present invention is a preparative liquid chromatograph for separating and extracting components in a sample, the preparative liquid chromatograph including a separation channel through which a mobile phase flows, an injector that injects the sample into the mobile phase, a separation column for separating components in the sample injected into the mobile phase, the separation column being provided downstream of the injector on the separation channel, a detector for detecting peaks of the components separated by the separation column, a fraction collector configured to collect an eluate from the separation column into a plurality of collection containers at a downstream of the detector while fractionating the eluate, and a controller for controlling operation of the fraction collector, wherein the fraction collector is provided with a peak collection containers and waste liquid collection containers, each peak collection container is used for collecting a peak portion including a collection target peak detected by the detector in the eluate, and the waste liquid collection container is used for collecting a waste liquid portion not including the collection target peak in the eluate, and the controller is configured to collect the peak portion including the collection target peak detected by the detector in the eluate in the peak collection container, and to collect at least a part of the waste liquid portion in the waste liquid collection container.

In a first aspect of the first embodiment, the controller is configured to require a user to designate, on a chromatogram of the sample acquired in advance, at least one collection target peak to be collected in the peak collection container, and is configured to collect at least one peak portion each including the at least one collection target peak designated by the user in the peak collection container and waste liquid portions before and after the at least one peak portion in the waste liquid collection container. According to such an aspect, the collection target components flowing before and after the peak portion collected in the peak collection container can be collected without significant dilution.

In the first aspect, the controller may be configured to require a user to designate an amount of each of the waste liquid portions to be collected before and after the at least one peak portion in the waste liquid collection container. This allows the user to optionally set how much the waste liquid portions before and after the peak portion are collected according to a chromatogram or the like acquired in advance.

In a second aspect of the embodiment, the controller is configured to collect all of the waste liquid portion in the waste liquid collection container after separation and extraction, which is started by injecting a sample into the mobile phase, of the sample is started until the separation and extraction are completed. As a result, even when there is a mistake in setting the sorting condition, because the entire waste liquid portion is collected in the waste container collection container, it is possible to prevent loss of valuable sample and the waste liquid portion can be reused.

DESCRIPTION OF REFERENCE SIGNS

2: separation channel4: liquid feeding pump6: injector8: separation column10: detector12: fraction collector14: controller16: probe18: switching valve20: peak collection container22: waste liquid collection container