JPH08160052A - Automatic sample preparation device for analysis - Google Patents

Abstract

PURPOSE: To execute sampling adjustment work at chemical analysis easily and surely by automatically sampling after a specified time passed when reaction is started with the liquid in a reaction container. CONSTITUTION: For preparing a base starch liquid, measured wheat starch is provided in a reaction container 21 along with acetic acid buffer liquid, so that, an automatic control device of a control panel 2 starts operation for agitation with a mixer. Then, measurement amylase liquid is poured in the container 21 for agitation, so that, hydrolysis is started, and at this time, a switch of a time adjusting device is turned on. Meanwhile, the automatic control device works for adjusting hot water quantity, and a magnetic stirrer is activated for keeping the temperature in the container 21 at 30 deg.C. When a specified time has passed, the automatic control device works so that a piston up/down device 8 works, and a syringe 3 automatically sucks up sample liquid 20 in the container 21 through a filter 24, for sampling. Thereby, in the sampled liquid, reaction does not progress, so that reaction state after the specified time period is kept.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an automatic sample preparation device for chemical analysis used in chemical analysis.

[0002]

2. Description of the Related Art Sample preparation work in chemical analysis is a very important work. For example, in the case of a reaction with a reagent for component analysis or component detection, generally, a liquid to be analyzed is directly or diluted, and a reagent is added while keeping a constant temperature while keeping a constant temperature and sufficiently stirred to react. Further, a part of this is taken out and the means for advancing to the next reaction is repeated to obtain the desired result. In this work, it is rare that the result at the intermediate stage of the reaction is required. This is because it is general to adjust the amount of reagents to be introduced so that the reaction can be sufficiently performed. Also, when the reaction time is limited, the reaction termination treatment (for example, neutralization is performed at the limited time). It is usually done by adding another reagent or stopping the reaction). Because, in such work, even if the sample liquid in the reaction is extracted with time, the reaction will proceed in the extracted liquid and the reaction will not stop due to sampling. These automations were not very effective because they had to be done after the outage. That is, simply performing the automatic sample withdrawal after a certain period of time did not limit the reaction time. Therefore, it was rare to sample accurately after the passage of time.

The inventors of the present invention have separately made several inventions regarding a method for measuring the amount of maltose using a flow injection analysis method. For example, the method described in Japanese Patent Application No. 6-22323 measures the amount of maltose produced by the digestive action of amylase on starch. The digestion time is kept constant when amylase is added to the starch solution. The amount of maltose that is generated is calibrated. That is, it is necessary to keep the digestion time constant, and it is necessary to stop the reaction after a certain period of time. The starch can be removed. If the undigested starch is not contained, digestion is not performed even if amylase is contained in the reaction solution, so the reaction of the original solution is stopped. As described above, the reaction may be substantially stopped when the reaction solution is taken out through the filter in the sample preparation for analysis. In this case, an apparatus for stopping the reaction time by automatic suction after a lapse of a certain time is needed. Further, since the reaction is substantially stopped by the filter, there is an advantage that it is not necessary to immediately start the next analysis work even after the reaction time has elapsed.

In the method for measuring amylase activity using the flow injection analysis method by the present inventor, in order to prepare a base starch solution, wheat starch is weighed and put in a reaction vessel, a buffer solution is injected, and a mixer is used to sufficiently prepare the starch solution. After stirring, the prepared enzyme solution containing amylase is put into a reaction vessel and stirred to start hydrolysis. This time is set as the decomposition start time, and while the temperature of the sample solution in the reaction container is maintained at 30 ° C., 10 minutes after the start of hydrolysis, the sample solution in the reaction container is sampled through the filter by the syringe.

As described above, in this sample preparation work, it is necessary to mix the chemicals, stir them, maintain them at a constant temperature, and sample them after a predetermined time. It is a troublesome work to carry out this reliably by hand. It has been conventionally desired to automate this.

[0006]

SUMMARY OF THE INVENTION The present invention has been made in view of the above points, and provides an automatic sample preparation method and apparatus for chemical analysis that can automatically perform sample preparation work in chemical analysis. With the goal.

[0007]

In order to solve the above-mentioned problems, the present invention provides a reaction container for putting and stirring a reaction liquid, a syringe for automatically sampling the liquid in the reaction container, and a reaction container. It consists of a heat insulation device that keeps it at a constant temperature,
It is characterized in that the sample is sampled after a lapse of a certain time after the start of the reaction by using a time measuring device. Further, the present invention is characterized in that the piston of the syringe is automatically sampled by a piston up-and-down device which slides the piston relative to the cylinder. Further, the present invention is characterized in that a mixed solution of starch solution and amylase is used as a reaction solution, and a sample is prepared through a filter at the tip of the syringe.

[0008]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An automatic sample preparation device for chemical analysis of the present invention will be described below with reference to the drawings.

FIG. 1 is a diagram for explaining the schematic configuration of an automatic sample preparation device for chemical analysis according to the present invention.

The case where the present invention is used for measuring amylase activity using the above-mentioned flow injection analysis method will be described.

The automatic sample preparation device for chemical analysis shown in FIG. 1 is mounted on a horizontal mounting plate 13 fixed to an underframe 11, a magnetic stirrer 12 mounted thereon, and a magnetic stirrer 12. A reaction container 21, a syringe 3 composed of a cylinder 4 and a piston 5 suspended in the reaction container 21, a piston elevating device 8 for performing a sampling action on the syringe 3, a box 10 surrounding the piston elevating device 8, and a box body A horizontal support plate 6 having 10 fixed to the upper surface,
The support plate 6 is provided with devices such as a column 14, a spring 15, a screw rod 16, a nut 19, and knurled knobs 17 and 18 for moving the support plate 6 up and down and fixing it at a constant height.

The magnetic stirrer 12 is a stirrer using electromagnetic force, and iron pieces are put in the reaction vessel 21 and rotated by a rotating magnetic field, and the starch in the reaction vessel 21 placed on the magnetic stirrer 12 is stirred. Stir liquid etc.

The reaction vessel 21 is made of double-walled glass and contains the sample solution 20 in which the starch solution and the amylase solution are mixed and stirred. Hot water flows from the inlet 22 between the double walls and is discharged from the outlet 23, so that the sample solution 20 is maintained at an appropriate temperature. The syringe 3 is suspended in the reaction container 21. The syringe 3 is a cylindrical cylinder 4
And a piston 5 sliding therein, a filter 24 is attached to the lower end of the cylinder 4, and the inflow pipe 1 is connected to the lower end thereof. As will be described later, when the piston 5 is pulled up from the cylinder 4, the reaction container 2
The sample liquid 20 in 1 is sucked.

A horizontal mounting plate 13 fixed to the underframe 11.
The column 14 is fixed to the upper surface of the upright. A horizontal support plate 6 that slides up and down along the column 14 is provided, and the magnetic stirrer 12 and the reaction vessel 21 are arranged between the horizontal support plate 6 and the horizontal mounting plate 13. Has become. The support plate 13 has an appropriate height and supports 44
A knurled knob 18 is provided so as to be fixed to the. A compression spring 15 is arranged around the column 14 between the upper surface of the mounting plate 13 and the lower surface of the support plate 6, and the support plate 6 is pressed upward by the compression spring 5.

A box 10 is fixed to the upper surface of the support plate 6. The column 14 penetrates the support plate 6 and projects into the box body 10, and is connected to the screw rod 16 by a nut 19.
The screw rod 16 protrudes upward from the upper wall of the box body 10, and the knurled knob 17 is screwed therein, and the lower surface of the knurled knob 17 is in contact with the upper wall surface of the box body 10. Therefore, if the knurled knob 18 is loosened and the knurled knob 17 is rotated, the support plate 6 and the box body 10 can be slid up and down along the column 14, and their heights can be adjusted.

A piston up / down device 8 is mounted in a box 10. The piston raising / lowering device 8 is composed of, for example, a nut that is screwed to a screw shaft or a pinion that meshes with a rack, and a piston holding member 7 that is fixed to these nuts and pinions. The piston raising / lowering device 8 is connected to a motor 9 by an interlocking device such as a gear or a chain and is driven by this. The piston holding member 7 moves in the vertical direction, and the head of the piston 5 of the syringe 3 can be detachably held. The cylinder 4 of the syringe 3 is detachably held by the support plate 6.

In FIG. 1, A indicates the moving distance of the piston holding member 7, that is, the stroke of the piston 5.
B is the distance from the upper surface of the support plate 6 to the nut 19,
By further raising the support plate 6 by the distance B, the entire syringe 3 can be removed from the reaction container 21. C is the height from the upper surface of the mounting plate 13 to the upper surface of the support plate 6, and indicates the mounting lower limit position of the syringe 3. When the support plate 36 is lowered below this, the inflow pipe 1 of the syringe 3 is supported on the inner bottom of the reaction container 51, and the operation becomes impossible.

A timing device is connected to the motor 9, and by operating this control device on the control panel 2 of the underframe 11, it is possible to control the operation time of the piston up / down device 8, that is, the sampling suction time by the syringe 3. . Also,
By operating the control panel 2, it is possible to control the flow rate of the hot water in the reaction vessel 21, and thus the temperature of the sample solution 20 in the reaction vessel 21.

The automatic sample preparation device for chemical analysis of the present invention having the above-described structure operates as follows.

In the amylase activity measurement using the flow injection analysis method, wheat starch is weighed and put into the reaction vessel 21 to prepare a base starch solution, and an acetate buffer solution is injected. At this point, the automatic control device of the control panel 2 starts to operate. Stir them thoroughly with a mixer. The amylase solution to be measured prepared in a test tube is placed in the reaction vessel 21.
When the mixture is put in and stirred, hydrolysis starts. Since this time is the hydrolysis start time, switch on the time limiter. During this time, an automatic control device works by the control panel 2 to adjust the amount of hot water and activate the magnetic stirrer to keep the temperature in the reaction vessel at 30 ° C. When the set predetermined time has elapsed after the start of hydrolysis, the automatic control device of the control panel 2 operates to operate the piston up / down device 8, and the syringe 3 causes the filter 2 to move.
The sample solution 20 in the reaction container 21 is automatically sucked through the sample 2 and sampled. As a result, the sampled liquid does not proceed with the reaction and becomes a sample in which the reaction state is maintained for the required time.

While the above examples have been described as using the present invention for measuring amylase activity using flow injection analysis, it can be used for other chemical analyses. Also, by setting a plurality of these devices together and operating them with one control device, it is possible to perform measurements with different reaction times, and if different types of samples are prepared, several types of samples can be made at once.

[0022]

As described above, in the method and apparatus of the present invention, a chemical analysis sample or the like is placed in a reaction container, and the liquid after the reaction in the reaction container after a certain time is automatically sampled. Since it is configured as described above, there is an effect that the sample preparation work at the time of chemical analysis can be carried out easily and surely.

[Brief description of drawings]

FIG. 1 is a diagram illustrating a schematic configuration of an automatic sample preparation device for chemical analysis according to the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Inflow pipe 2 Control board 3 Syringe 4 Cylinder 5 Piston 6 Support plate 7 Piston holding member 8 Piston up-and-down device 9 Motor 10 Box body 11 Underframe 12 Magnetic stirrer 13 Attachment plate 14 Strut 15 Compression spring 16 Screw rod 17 Knurled knob 18 Knurled knob 19 Nut 20 Sample liquid 21 Reaction vessel 22 Hot water inlet 23 Hot water outlet 24 Filter

Claims (3)

[Claims] 1. A reaction vessel for containing and stirring a reaction solution, a syringe for automatically sampling the solution in the reaction vessel, and a heat-retaining device for keeping the reaction container at a constant temperature. An automatic sample preparation device for chemical analysis, characterized in that a sample is prepared after a lapse of a certain time after the start of the reaction. 2. The automatic sample preparation device for chemical analysis according to claim 1, wherein the piston of the syringe is automatically sampled by a piston lifting device which slides relative to the cylinder. 3. The automatic amylase reaction according to claim 1 or 2, wherein a sample solution is prepared by using a mixture of starch solution and amylase as a reaction solution and passing through a filter at the tip of the syringe. Sample preparation device.