JPH08271490A - Dispenser for liquid chromatography - Google Patents

Abstract

PURPOSE: To enhance the operating rate of liquid chromatograph by enhancing the operating rate of a dispenser. CONSTITUTION: A comparing section 2 prolongs the sampling interval, being set as an initial value, sequentially by an unit time until the overlapped operation of pipeter is avoided. An inhibition area memory 4 stores the operating time of pipeter for each sample as an inhibition area. A comparing section 2 determines a sampling interval such that the operating time of pipeter for each sample is not overlapped over the inhibition area of other sample stored in that inhibition area memory 4.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dispensing device called an autosampler for automatically injecting a sample into a high performance liquid chromatograph, and more particularly to a sample container for accommodating a plurality of samples and a reagent accommodating a plurality of reagents. A reagent storage part for
A reaction container accommodating part for accommodating a plurality of reaction containers, a cleaning part, a needle is moved to each part by an arm mechanism,
A liquid is sucked and discharged by the needle to dispense a sample and a reagent into a reaction container, and a sample solution after the reaction is sucked from the reaction container and injected into an injector of a liquid chromatograph, and the needle is also washed 1 The present invention relates to a pipetting apparatus provided with individual pipettors and a control unit that controls the pipettors according to a pipetter operation time and a stationary time that are determined by analysis conditions.

[0002]

2. Description of the Related Art A dispenser for injecting a sample into an injector of a liquid chromatograph is equipped with a single pipettor, dispenses a sample and a reagent into a reaction container and causes them to react, and the sample solution after the reaction is injected into the injector. There is a method of injecting into. The sample dispensing operation by such a dispensing device is performed, for example, as shown in FIG. 1
Dispense the first reagent into the reaction vessel for the second sample,
After the standing time, the sample was dispensed into the reaction vessel,
Stir and let stand for a period of time. After that, the second reagent is dispensed into the reaction container, stirred, and allowed to stand for a certain period of time again. After that, suction the sample solution after reaction with a pipette,
Inject into the injector of the liquid chromatograph. When injected into the injector, the sample components are separated by the column and analyzed. The time during which the pipettor is operating, such as dispensing reagents and samples and injecting the sample solution after the reaction into the injector, is called the pipetter operating time.The time during which the pipetter is stationary and the sample reacts with the reagent is called It is called stationary time, and the time from the injection of the sample solution into the injector to the end of the analysis of the sample is called the analysis time.

Since only one pipettor is provided, when the dispensing operation of the next sample is started between the start of dispensing one sample and the end of analysis, the pipetting operation time overlaps between the two samples. In this case, the dispensing operation cannot be performed. Although the pipetter operation time and the standing time vary depending on the analysis conditions, in the past it was not possible to find the overlap of the pipettor operation time when the dispensing operation of two or more samples proceeded in parallel. So that 1
The dispensing operation of the next sample is started after the analysis time of one sample is completed.

[0004]

Since the dispensing operation of the next sample is started after the analysis time of one sample is finished, there arises a problem that the operation rate of the liquid chromatograph becomes low. An object of the present invention is to increase the operation rate of a liquid chromatograph by increasing the operation rate of a dispensing device.

[0005]

[Means for Solving the Problems] The pipette operation time required by each instruction for operating the pipettor of a pipetting apparatus is obtained from analysis conditions, and the pipetting start time of each sample is shifted by sample intervals of equal time intervals, When the pipetting operations of two or more samples are performed in parallel, the minimum sample interval at which the pipette operation time of each sample does not overlap is found,
The dispensing operation is performed by the dispensing device at the sample interval. As an example, the dispensing operation shown in Table 1 will be described.

[0006]

[Table 1]

JOBA to D are pipetter operation times in which the pipettor operates to perform reagent dispensing, sample dispensing, and injection into the injector, and WAITa to c are WAITa to c in which the pipetter is stationary and the dispensed reagent or sample is a reaction container. WAITd is the analysis time from the injection of the sample solution into the column to the end of the analysis.

A case will be described in which this series of dispensing operations is sequentially started at a constant sample interval a for five samples. As shown in FIG. 2, the dispensing of each sample is started while shifting the sample interval a by time, and the sample interval a is determined so that the pipette operation time does not overlap, and the dispensing operation is performed accordingly. To perform.

Therefore, the control unit 1 has the functions of the respective units shown in FIG. The comparison calculation unit 2 performs calculation so that the sample interval a set as the initial value is lengthened by unit time until overlapping of pipette operation times is avoided. The prohibited area memory 4 stores the pipette operation time of each sample as a prohibited area.
Is to determine the sample interval a so that the pipette operation time of each sample does not overlap with the prohibited areas of other samples stored in the prohibited area memory 4.

An example of the operation will be described with reference to the flowchart of FIG. At the start of the program, the pipette operation time, static time, and analysis time determined by the analysis conditions are taken in as the initial conditions, and i = (total time of all jobs / maximum number of jobs that can be processed) as the initial value of the variable i of the sample interval a. Or, set the maximum value of (JOBA time) or (WAITd time). The program for obtaining the sample interval a is to increase the initial value i by unit time until the pipette operation time does not overlap with five samples.

First, the initial value of the sample interval a is set to 0. As the sample number P0 for checking the overlap of the pipette operation time, the larger one of P0 = ((total time of all jobs) / i + 1) or (total number of samples) is adopted. The initial value of the number of samples P to be compared is set to 0. Further, the initial value of K indicating the job number of each sample is set to 0 (steps S1 to S
4).

After storing the pipetter operation time of the first sample in the prohibited area, in order to obtain the start time B and the end time E of the Kth job for the second sample, B = dispensing start of that sample To the start of the Kth job + a E = time from the start of dispensing of the sample to the end of the Kth job + a is calculated, and the pipetter operation time B of the Kth job B to
It is checked whether or not E overlaps the prohibited area obtained so far (steps S5 to S7). If they overlap, unit time is added to the sample interval i and steps S1 to S7 are repeated (steps S8 to S10).

If the pipette operation time of the Kth job and the prohibited area do not overlap, it means that there is no overlap with the pipette operation time of the previous samples until the Kth job of the sample. K is incremented by 1 and the next job is examined (steps S8 and S1).
1, S12). In this way, one sample is examined up to the fourth job, and if the pipette operation times do not overlap, the pipette operation times B to E for that sample are added to the prohibited area (step S1).
3) The variable i of the sample interval thus obtained is added to the sample interval a previously obtained, and 1 is added to P to similarly obtain the sample interval at which the pipette operation time does not overlap (steps S14 and S15). . If P = P0, it means that all the samples have been examined, and the determined a is the sample interval (step S1).
6).

In step S8, the pipette operation time overlaps the prohibited area, and unit time is added to i. When i becomes (total time of all jobs) or more, two samples are processed in parallel. As a result, the pipette operation times do not overlap (step S10).

[0015]

FIG. 5 is a schematic plan view of the mechanical portion of one embodiment. A plurality of sample vials are arranged in the sample rack 10, and the reaction vial rack 12
A plurality of empty reaction vials are placed in the. The sample and the reagent are dispensed into the reaction vial to carry out the reaction. A plurality of reagent vials 16r for each item are arranged in the reagent vial rack 16. A washing port 17 for washing the needle and a drain port 19 for discarding the drainage are arranged outside the rack. A column thermostat 14 accommodating a high performance liquid chromatograph column is disposed between the sample rack 10 and the reaction vial rack 12, and the column thermostat 14 is provided with an injector 18 for injecting the sample solution into the column. Has been.

A needle 20 for sucking and discharging a sample or a reagent is attached to a vertical arm 22 which moves the needle 20 in a vertical direction (Z direction perpendicular to the paper surface), and the vertical arm 22 extends in a Y direction. Can be moved in the Y direction. Horizontal arm 24
Can move in the X direction along a guide rail 26 extending in the X direction. By these arms 22 and 24, the needle 20 moves the position of any sample vial of the sample rack 10, the position of any reaction vial of the reaction vial rack 12, and the position of any reagent vial 16 r of the reagent vial rack 16 and the washing port 17. , Can be moved to the position of the drainage port 19. Needle 2
0 is connected to a suction / discharge mechanism for sucking and discharging liquid.

When performing the four pipettor operations shown in Table 1, the needle 20 moves to the reagent vial rack 16 to aspirate the first reagent and dispense it into one reaction vial of the reaction vial rack. Next, the needle 20 moves to a position of a predetermined sample vial of the sample rack 10, sucks the sample, and dispenses the sample into the reaction vial. Then, the needle 20 moves to the reagent vial rack 16 to suck the second reagent and dispense it into the previous reaction vial. Then, the reaction solution in the reaction vial is injected into the injector 18. After dispensing the sample and reagent, the needle 20 moves to the drainage port 19 to discard the excess liquid, and the washing port 17
Move to and wash. The present invention is not limited to the dispensing device shown in FIG. 5, but can be similarly applied to a system in which samples and reagents are transferred by a turntable.

[0018]

According to the present invention, in a pipetting apparatus provided with only one pipettor, a plurality of samples can be injected in parallel to the injector at the shortest sample interval depending on the analysis conditions of the sample and the number of samples. All samples can be dispensed in the shortest time, improving the operation rate of the liquid chromatograph.

[Brief description of drawings]

FIG. 1 is a time chart showing a conventional dispensing operation.

FIG. 2 is a time chart showing a dispensing operation required by the present invention.

FIG. 3 is a block diagram showing a function of determining a sample interval in one embodiment.

FIG. 4 is a flowchart illustrating the operation of one embodiment.

FIG. 5 is a schematic plan view showing an embodiment.

[Explanation of symbols]

 1 Control Section 2 Comparison Calculation Section 4 Prohibited Area Memory 10 Sample Rack 12 Reaction Vial Rack 14 Column Constant Temperature Bath 16 Reagent Vial Rack 18 Injector 20 Needle 22 Vertical Arm 24 Horizontal Arm

Claims (1)

[Claims] 1. A sample container for accommodating a plurality of samples, a reagent container for accommodating a plurality of reagents, a reaction container container for accommodating a plurality of reaction containers, a washing unit, and an arm mechanism for connecting a needle to said needle. The sample and reagent are dispensed into the reaction container by suctioning and discharging the liquid with the needle, and the sample solution after reaction is sucked from the reaction container and injected into the injector of the liquid chromatograph, and the needle In the pipetting device comprising one pipettor which also cleans the pipette, and a control unit which controls the pipette according to a pipetting time and a standing time determined by analysis conditions, the pipette of the pipetting device operates in the control unit. The pipette operation time required for each command is obtained from the analysis conditions, and the dispensing start time of each sample is shifted by sample intervals of equal time intervals, and is set to 2 or more. When the sample dispensing operations of are performed in parallel, the minimum sample interval at which the pipette operation time of each sample does not overlap is found, and the dispensing operation is executed at the sample interval. Liquid chromatograph dispensing device.