JPH02238359A - Sample injection device with preparative separation function - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a device called an autosampler or an autoinjector, which automatically introduces a sample into a liquid chromatograph.

(Prior art) An autosampler holds multiple samples, sucks in the selected sample with a needle, and injects it into the sample injection port of a liquid chromatograph. In addition to simply injecting the sample from the sample bottle, some models are equipped with a reagent bottle and have the function of mixing the sample and reagent, performing pretreatment, and then injecting the sample into the injection port. In liquid chromatography, a sample is separated and detected, and then each component is fractionated. To perform fractionation automatically, a fractionation system called a fraction collector is used.

(Problems to be Solved by the Invention) In order to automatically perform sample injection and fractionation in a liquid chromatograph, it is necessary to have two devices: an autosampler and a fraction collector. The purpose of the present invention is to reduce costs and downsize the device by equipping an autosampler with a preparative collection function and realizing two functions of sample injection and preparative collection with one device. be.

(Means for Solving the Problems) In the present invention, a separation port is provided in a flow path downstream of a detector of a liquid chromatograph. This fractionation port has a volume necessary for fractionation, and is equipped with an outlet at the lower end that is opened and closed by a solenoid valve. A needle can be moved to this preparative collection port, and the sample is drawn in through the needle to perform preparative collection.

(Function) When injecting a sample into the sample injection port, the function is similar to that of a conventional autosampler.The needle inhales the sample from the sample bottle, mixes it with a reagent if necessary, and then injects the sample into the sample injection port. inject.

During analysis using a liquid chromatograph, leave the outlet at the bottom of the preparative port open, and when the detector detects a component to be separated, close the outlet at the bottom of the preparative port and move the needle up to the port. Move and aspirate the effluent collected in the preparative port. When inhalation is complete, open the outlet, move the needle to a suitable container such as an empty bottle, and inject the inhaled effluent. (Example) Figure 1 schematically represents an example. Second
The figure shows a separation port in one embodiment, and FIG. 3 is an external perspective view of one embodiment. 2 is a sample rack in which a plurality of sample bottles 4 are arranged. Also arranged in the sample rack 2 are empty bottles 6 for use in mixing samples and reagents, and for holding fractionated effluents.

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 diluent.

Further adjacent to the sample rack 2, an injection port 12,
A separation port 14 and a washing port 16 are arranged.

A needle 18 is provided above the sample bottle 4, the reagent bottle 10, and each port 12, 14, 16.

The holder 20 holding the needle 18 is a guide 22
The guides 22 and 24 are respectively supported so that they can be moved in the Z direction, the guides 22 are movable in the X direction along the guides 24, and the guides 24 are movable in the Y direction. The movement in each direction is automatically controlled, and the sample bottle 4, reagent bottle 10, each port 12, 14, 16
The needle 18 can be moved to any position. The other parts except the preparative port 14 are already in practical use as an autosampler. As shown in FIG. 1, injection port 12 is connected to a six-way valve 26. The six-way valve 26 further includes a sample loop 28.
, column 30, eluent supply channel 32 and drain channel 3
4 is connected. A plurality of solvents 38a to 38c can be mixed and supplied at a predetermined ratio from the flow path 32 by a pump 36 and a solenoid valve (not shown). A detector 40 is connected to the outlet of the column 3o, and a separation port 14 is connected to the outlet of the detector 40. The outlet port 14 has an inlet 14a connected to the detector and an outlet 1 connected to the drain on the side wall, as shown in FIG.
4b, a discharge port 14c is provided at the lower end, and a space 42 having a volume necessary for fractionation is formed inside.

The upper end of the separation port 14 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 separation port, and opening and closing operations of the solenoid valve 46 are controlled based on a detection signal from the detector 40.

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

Next, the operation of this embodiment will be explained.

The six-way valve 26 is positioned at the position shown by the solid line in FIG. 1, and the eluent is supplied from the pump 36. A needle 18 aspirates a sample from a predetermined sample vial 4 and injects it into the injection port 12 . When it is necessary to mix the sample with the reagent, empty the bottle 6.
After the sample and reagent are injected into the nozzle 18 and mixed by suction and discharge through the nozzle 18, the mixed solution may be injected into the injection port 12. A sample injected into injection port 12 is collected into sample loop 28 . After the injection of the sample is completed, the needle 18 is inserted into the cleaning port 16 and cleaned.

Next, the six-way 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 and enters the column 3o, where it is separated and sequentially detected by the detector 40.

The sorting operation will be explained with reference to FIG.

The solenoid valve 46 is open until the fractionation is started (step SL).

When the detector 40 detects a component to be separated, the solenoid valve 46
is closed (steps S2, S3). Then, the needle 18 moves to the preparative port 14 position, and the preparative port 14
After the needle 18 is inserted into the syringe and the effluent is inhaled by the syringe, the needle 18 moves to the position of the empty bottle 6 and injects the inhaled liquid into the empty bottle 6 (steps S4 and S5). When the solenoid valve 46 is closed, the effluent flows into the space 42 of the preparative port 14.
When the volume exceeds , the effluent is discharged from the discharge port 14b to the drain.

When the preparative separation is completed according to a signal from the detector 40 (step S6), the W1 magnetic valve 46 is opened (step S7).
, the needle 18 is moved to the cleaning port 16 and cleaned (step S8).

Thereafter, 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 bottles 4 are placed on the sample rack 2, the present invention can also be applied to an autosampler in which the sample bottles are placed on a turntable. (Effects of the Invention) In the present invention, the sample injection device is equipped with a preparative port so that sample injection and preparative separation can be performed automatically with one device.
Costs are lower and the equipment can be made smaller.

[Brief explanation of drawings]

Fig. 1 is a schematic configuration diagram showing one embodiment, Fig. 2 is a cross-sectional view showing the separation port of the embodiment, Fig. 3 is an external perspective view showing the -embodiment, and Fig. 4 is a schematic diagram showing the separation port of the embodiment. FIG. 3 is a flowchart diagram showing a sorting operation. 4...Sample bottle, 12...Injection port,
14...Preparation port, 18...Needle, 30...Column, 40...Detector, 42...Preparation port Space, 46...
·solenoid valve. Patent applicant: Shimadzu Corporation

Claims (1)

[Claims] (1) A sample injection device that holds multiple samples, inhales the selected sample with a needle, and injects it into the sample injection port of the liquid chromatograph, which is connected to the flow path downstream of the detector of the liquid chromatograph and placed in a predetermined position. It has a volume of
A sample injection device characterized in that the needle is inserted into the preparative port to collect the sample.