JPS638555A - Fast liquid chromatograph - Google Patents

Abstract

PURPOSE:To set eluting conditions suitable for a desired component independently, by switching columns while supplying a mobile phase suited to the elution of the desired component to a plurality of columns. CONSTITUTION:When feed pumps 4 and 11 are operated to inject a sample into a sample injection port 5, a sample flows into an analysis column 2 by a first mobile phase to hold a elutable component alone. When a second passage is formed by an changeover valve 9, a component not held by the first mobile phase flows into a second analysis column 9. The desired component shifted to the second analysis column 9 is eluted by a second mobile phase to be held by a second analysis column 9. This keeps the flow rate ratio between the first and second moving layers, which flow into a liquid mixing means 8 from a branch tube 7, constant even at the switching of these passages and causes the layers to be mixed thoroughly, thereby eliminating hourly variations in the background noise of a detector 12.

Description

DETAILED DESCRIPTION OF THE INVENTION A. Field of Industrial Application The present invention relates to a high-performance liquid chromatography system suitable for analyzing samples containing a plurality of target substances under different elution conditions.

Conventional technology When analyzing samples containing components with significantly different elution conditions using a high-performance liquid chromatography device, prepare multiple types of solvents suitable for elution of each target component, and adjust the mixing ratio of each solvent over time. A gradient elution method is used in which the target component is dissolved by changing the concentration.

However, since the mixing ratio of multiple solvents constituting the mobile phase is changed over time, it not only requires skill to set the analysis conditions, but also the background of the output of the modeler due to the change in the solvent over time. Since the noise also varies over time, it becomes difficult to detect the peak of the image component, making it unsuitable for high-sensitivity analysis.

Generally speaking, when a plurality of samples are analyzed continuously, it is necessary to remove the mobile phase in the column and return it to the initial state, which poses the problem of prolonging the measurement cycle.

C. Purpose The present invention was made in view of these problems, and its purpose is to improve analytical sensitivity and shorten measurement cycles by stabilizing background noise. The object of the present invention is to provide a high-performance liquid chromatography device.

21. Structure of the Invention, that is, the present invention is characterized in that it is possible to switch between columns while supplying a mobile phase suitable for elution of a target component to a plurality of columns.

E. Embodiments The details of the present invention will be explained below based on illustrated embodiments.

FIG. 1 shows one embodiment of the present invention, and reference numeral 1 in the figure is a switching valve consisting of a high-pressure six-way valve, which switches between the first and second analysis channels, which will be described later. 2 is
The inlet of the first analysis column for high-performance liquid chromatography is connected via the sample injection port 5 to the discharge port of the first liquid feed pump 4, which communicates with the mobile phase liquid tank 3 regardless of the flow path. ing. On the other hand, the outlet is connected to a liquid mixing means 8 such as a mixing coil through a resistance tube 6 and a branch pipe 7 when forming the first flow path (solid line in the figure), and when forming the second flow path (solid line in the figure). The dotted line in the figure) is connected to the inlet of a second analytical column 9 for high performance liquid chromatography, which will be described later. 9 is the aforementioned second analysis column, the outlet of which is connected to the mixing coil 8 via the branch pipe 7 regardless of the flow path;
Further, the inflow port is connected to the discharge port of the liquid feeding pump 11 that communicates with the mobile phase liquid tank 10 when the first flow path is formed, and
When forming the flow path, the outlet of column 2 is connected. On the other hand, the discharge port of the second liquid pump 11 is connected to the mixing coil 8 via the resistance tube 6 when forming the second flow path.
be done. Note that the reference numeral 12 in the figure indicates a detector connected to the outlet of the mixing coil 8.

In this example, each mobile phase tank 3.10 contains a solvent capable of eluting each target component of the sample;
Furthermore, when the switching valve 1 is operated to form the first flow path, the first liquid feeding pump 4 → the sample injection port 5 → the first analysis column 2
A flow path →resistance tube 6 →mixing coil 8 and, separately from this, a flow path such as second liquid feeding pump 11 →second analysis column 9 →mixing coil 8 are formed.

When such preparations are completed, each liquid pump 4.11 is activated to inject the sample/pull into the sample injection port 5, and the sample flows into the analytical column 2 of the column 1 by the first mobile phase. Only components that can be eluted by the first mobile phase are retained in the first analytical column 2, while other components that cannot be retained by the first mobile phase remain in the first analytical column 2. It will be discharged from now on. At this point of discharge, switching valve 1
When the outlet of the first analytical column 2 is connected to the second analytical column 9 by forming a second flow path, the components not retained by the first mobile phase are absorbed together with the first mobile phase. 2
into analytical column 9. When all the components not retained by the first mobile phase have flowed into the analytical column 9, the switching valve 1 is operated again to form the first flow path. Needless to say, since the components that can be eluted by the first mobile phase are retained in the analytical column 2 of the food 1, they will not be discharged to the second analytical column 9.

By the way, even when these flow paths are switched, the flow rate ratio of the first and second mobile phases flowing into the liquid mixing means 8 from the branch pipe 7 is kept constant, and the liquid mixing means 8 sufficiently mixes them. Therefore, the background noise of the detector 12 does not fluctuate over time.

The target component transferred from the first analytical column 2 to the second analytical column 9 is eluted by the second mobile phase and retained in the second analytical column 9. In this way, the target components retained in each analytical column 2.9 are separated by the mobile phase flowing into each column, and are removed from the column 2.9 after a retention time determined by the analytical conditions has elapsed. It is discharged together with the mobile phase. These discharged components are
The mobile phase flows into the liquid mixing means 8 via the branch pipe 7. Both mobile phases flowing into the liquid mixing means 8 are mixed here to form a homogeneous medium that transfers the components from each column to the detector 12.

As a result, the target component flows into the detector] 2 in a state mixed with a temporally constant medium, and forms a peak while being added to a constant background noise. Therefore, area and height can be detected extremely easily.

In this way, when all the components have been discharged from column 2.9, there will be enough mobile phase in column 2.9 to be used for analysis, so the next sample can be injected. This makes analysis possible.

In this example, the case where two types of mobile phases are used was explained. However, when three or more analytical columns are used, these columns can be connected in series using a switching valve, and each column can be moved differently. It is clear that by allowing the phase to be supplied, the present invention can also be applied to the analysis of samples containing three or more types of target components under different elution conditions.

Further, in this embodiment, a plurality of flow passages are formed using a switching valve, but it goes without saying that a combination of a three-way valve and a stop valve can provide the same effect.

In general, by setting the temperature N% of column 2.9 individually, more accurate and sensitive analysis becomes possible.

As explained above, in the present invention, a plurality of columns can be connected in series or in parallel, and when connected in series, a liquid pump is connected to the first column through a sample injection means. In addition, when connected in parallel, an independent liquid pump 78 was connected to the inlet of each column, while the outlet side was connected to the detection means via a common liquid mixing means.
Elution conditions suitable for target components can be set independently, which not only increases the degree of freedom in analysis conditions, but also keeps background noise constant by keeping the components of the mobile phase flowing into the detection means constant over time. This makes it possible to analyze trace amounts of components, and in general, at the end of the analysis, only the appropriate mobile phase is present in each column, eliminating the need for column initialization. As a result, the analysis cycle can be shortened.

[Brief explanation of drawings]

The figure is a configuration diagram of an apparatus showing an embodiment of the present invention. 1...Switching valve 2...Analysis column 3.
... Mobile phase liquid tank 4 ... Liquid pump 5 ...
Sample injection port 8...Liquid mixing means 9...Analysis column 10...Mobile phase liquid tank 11...Liquid pump

Claims (1)

[Claims] Multiple columns can be connected in series or in parallel, and when connected in series, a liquid pump is connected to the first column via a sample injection means, and when connected in parallel, an independent pump is connected to the inlet of each column. A high-speed liquid chromatography device in which a liquid sending pump is connected, and an outlet is connected to a detection means via a common liquid mixing means.