JPH0711513B2 - Sample injection device with preparative function - Google Patents

Description

TECHNICAL FIELD The present invention relates to an apparatus called an autosampler or an autoinjector, which automatically introduces a sample into a liquid chromatograph.

(Prior Art) An autosampler holds a plurality of samples and inhales a selected sample with a needle to inject it into a sample injection port of a liquid chromatograph. In addition to simply injecting the sample in the sample bottle, there is also one that is equipped with a reagent bottle and has a function of injecting the sample into the injection port after performing pretreatment by mixing the sample and the reagent.

In a liquid chromatograph, a sample may be separated and then separated for each component. A fractionation device called a fraction collector is used for automatic fractionation.

(Problems to be Solved by the Invention) In a liquid chromatograph, in order to automatically perform sample injection and fractionation, two devices, an autosampler and a fraction collector, must be provided.

An object of the present invention is to reduce the cost and downsize the apparatus by providing the autosampler with a preparative function and realizing the two functions of sample injection and preparative with one device. .

(Means for Solving the Problems) In the present invention, a preparative port is provided in the flow path downstream of the detector of the liquid chromatograph. This sorting port has a volume necessary for sorting and has a discharge port opened and closed by a solenoid valve at its lower end. Allow the needle to move to this sorting port, and suction by the needle to perform sorting.

(Operation) When injecting a sample into the sample injection port, it has the same function as a conventional autosampler. It inhales the sample from the sample bottle with a needle, mixes it with a reagent if necessary, and then inserts the sample into the sample injection port. Inject.

Keep the outlet at the bottom of the preparative port open during analysis by liquid chromatography, and close the outlet at the bottom of the preparative port when the detector detects the component to be fractionated, and move the needle to the preparative port. It moves and sucks the effluent stored in the collection port. When the suction is completed, the discharge port is opened, the needle is moved to a suitable container such as an empty bottle as shown in FIG. 1, and the sucked out liquid is injected.

(Embodiment) FIG. 1 schematically shows an embodiment. Second
The figure shows a sorting port in one embodiment, and FIG. 3 is an external perspective view of one embodiment.

A sample rack 2 has a plurality of sample bottles 4 arranged therein. An empty bottle 6 is also arranged in the sample rack 2 for use in mixing the sample and the reagent and for storing the separated effluent.

A reagent rack 8 is provided adjacent to the sample rack 2,
A plurality of reagent bottles 10 are arranged. The reagent bottle 10 contains, for example, a diluting solution.

An injection port 12, a preparative port 14, and a washing port 16 are further arranged adjacent to the sample rack 2.

A needle 18 is provided above the sample bottle 4, the reagent bottle 10, and the ports 12, 14 and 16. The holder 20 holding the needle 18 can move in the Z direction along the guide 22, the guide 22 can move in the X direction along the guide 24, and the guide 24 can move in the Y direction. Each of them is supported so that the movement in each direction is automatically controlled, and the sample bottle 4, the reagent bottle 10, each port 12, 14,
The needle 18 can be moved to any of the 16 positions. Other parts except the preparative port 14 are already put into practical use as an autosampler.

As shown in FIG. 1, the injection port 12 has a hexagonal valve 26.
It is connected to the. The hexagonal valve 26 further includes a sample loop 28, a column 30, an eluent supply channel 32 and a drain channel.
34 is connected. From the flow path 32, a plurality of solvents 38a to 38c can be mixed and supplied at a predetermined ratio by a pump 36 and a solenoid valve (not shown).

A detector 40 is connected to the outlet of the column 30.
The collection port 14 is connected to the exit of 40.

As shown in FIG. 2, the outlet port 14 is provided with an inlet 14a connected to the detector and a discharge port 14b connected to the drain on the side wall, and a discharge port 14c at the lower end, so that the volume necessary for sorting is kept inside. A space 42 is formed. Preparative port 14
The upper end of is closed by a septum 44, and a needle is inserted into the space 42 from above the septum 44 through the septum 44.

A solenoid valve 46 is provided at the discharge port 14c of the sorting port, and the solenoid valve 46 is controlled in opening / closing operation based on a detection signal from the detector 40.

The needle 18 is sucked and discharged by a syringe (not shown).

Next, the operation of this embodiment will be described.

The hexagonal valve 26 is positioned at the position shown by the solid line in FIG. 1, and the eluent is supplied from the pump 36. The needle 18 sucks the sample from a predetermined sample bottle 4 and injects it into the injection port 12. When it is necessary to mix the sample with the reagent, the sample and the reagent may be injected into the empty bottle 6, mixed by suction and discharge by the nozzle 18, and then the mixed solution may be injected into the injection port 12.
The sample injected into the injection port 12 is collected in the sample loop 28. When the injection of the sample is completed, the needle 18 is inserted into the washing port 16 and washed.

Next, the hexagonal valve 26 is switched to the position indicated by the broken line. The sample in the sample loop 28 is pushed out by the eluent, enters the column 30, is separated, and is sequentially detected by the detector 40.

The sorting operation will be described with reference to FIG.

The solenoid valve 46 is open until the sorting is started (step S1).

When the detector 40 detects the component to be separated, the solenoid valve 46 is closed (steps S2, S3). Then, the needle 18 moves to the position of the preparative port 14, is inserted into the preparative port 14 and sucks the effluent with the syringe, and then the needle 18 is replaced with the empty bottle 6.
The liquid that has been inhaled after moving to the position is injected into the empty bottle 6 (steps S4 and S5). When the effluent becomes larger than the volume of the space 42 of the fractionation port 14 when the solenoid valve 46 is closed, the effluent is discharged from the discharge port 14b to the drain.

When the signal from the detector 40 reaches the end of the fractionation (step S6), the solenoid valve 46 is opened (step S7), and the needle
18 is moved to the cleaning port 16 and cleaned (step S
8).

Then, the sorting operation is repeated according to the signal from the detector 40.

Although FIG. 3 shows an example of an autosampler in which the sample bottle 4 is arranged in the sample rack 2, the present invention can be applied to an autosampler in which the sample bottle is arranged in a turntable.

(Effects of the Invention) In the present invention, the sample injection device is provided with the preparative port so that the sample injection and the preparative process are automatically performed by one device.
The cost is reduced and the device can be downsized.

[Brief description of drawings]

FIG. 1 is a schematic configuration diagram showing an embodiment, FIG. 2 is a sectional view showing a preparative port of the embodiment, FIG. 3 is an external perspective view showing the embodiment, and FIG. 4 is a view showing the embodiment. It is a flowchart figure which shows a sorting operation. 4 ... Sample bottle, 12 ... injection port, 14 ... preparation port,
18 …… Needle, 30 …… Column, 40 …… Detector, 42 ……
Space of preparative port, 46 ... Solenoid valve.

Claims (1)

[Claims] 1. A sample injection device for holding a plurality of samples, and injecting a selected sample with a needle to inject it into a sample injection port of a liquid chromatograph, which is connected to a flow path downstream of a detector of the liquid chromatograph. A sample injection device having a predetermined volume, a lower end having a preparative port having a discharge port opened and closed by a solenoid valve, and inserting the needle into the preparative port for preparative dispensing.