JP2585740B2 - Automatic analyzers and reaction vessels - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to an automatic analyzer and a reaction vessel, and more particularly to an automatic analyzer and a reaction vessel suitable for stirring a liquid in the reaction vessel.

[Conventional technology]

In a conventional clinical automatic analyzer, when a sample and a reagent added to a reaction vessel are stirred, for example, Japanese Patent Laid-Open No. 57-82769 is used.
In general, mixing was carried out by inserting and stirring the same stirring rod into a reaction vessel positioned in the order stirring position as shown in the above item. However, it is difficult for such a stirring method to completely remove the carryover between the reaction solutions. Therefore, non-contact stirring of the reaction solution has been considered.

JP-A-57-42325 discloses a method in which a disk is provided on the inner peripheral side of a row of reaction vessels arranged on a turntable so as to come into contact with the outer walls of a plurality of reaction vessels, and the disc is reciprocated to move the reaction vessel. 3 shows a mixing method of driven rotation.

On the other hand, although it is a stirrer without the function of an analyzer, Japanese Patent Application Laid-Open No. 52-143551 discloses that a large number of diluent chambers are formed in a rectangular plastic plate in the X and Y directions, and the plate is vibrated horizontally. Shows how to stir the liquid by giving In this example, in consideration of the fact that complete stirring cannot be performed only by simple vibration, one end of the plate is supported by a column, and an electromagnet or the like is operated to apply an arc-shaped vibration to the plate.

Japanese Patent Application Laid-Open No. 61-56972 discloses a spectrophotometer in which a cell holder in which a plurality of sample cells are set is linearly transferred, each sample cell is sequentially shifted to a measurement position, and after measurement, the spectrophotometer is returned to the cell holder and returned. In the figure, a normal rotation signal and a reverse rotation signal are alternately applied to the drive source of the cell holder to swing the sample cell back and forth, thereby stirring the sample.

[Problems to be solved by the invention]

In an automatic analyzer, since a large number of samples must be efficiently processed, a stirring operation without carryover between liquids to be stirred must be performed in a short time.

In JP-A-57-42325, the internal liquid can be stirred by rotating the reaction vessel itself, but the mechanism of the stirring device is complicated. Japanese Patent Application Laid-Open No. 52-143551 discloses a method of sequentially diluting a sample by inserting a diluting rod into each diluting liquid chamber one after another, and does not consider the effect of carryover during stirring. In Japanese Patent Application Laid-Open No. 61-56972, since the rectangular cell is only swung in the front-back direction, it takes a relatively long time for the liquid in the sample cell to be sufficiently mixed.

An object of the present invention is to provide an automatic analyzer capable of efficiently stirring a liquid in a reaction vessel with a simple configuration.

Another object of the present invention is to provide an automatic analyzer capable of promoting a reaction between a sample and a reagent by allowing repeated stirring during a period from addition of a sample and a reagent to measurement of a reaction solution. It is in.

Another object of the present invention is to provide an automatic analyzer capable of easily performing stirring without carryover between reaction solutions.

Another object of the present invention is to provide a reaction vessel which can enhance the effect of stirring the liquid and is easy to handle.

[Means for solving the problem]

In the present invention, the reaction vessel containing the stirring ball is arranged on the reaction disk, and the reaction disk is reciprocated at high speed in an arc shape to vibrate. The vibration causes the stirring ball in the reaction vessel to rotate, thereby causing the inside of the reaction vessel to rotate. The liquid was stirred.

[Action]

When the reaction disk is vibrated reciprocally in an arc shape under appropriate conditions, kinetic energy is given to a stirring ball submerged in a liquid in a reaction vessel arranged on the reaction disk. Accordingly, the stirring ball starts to move, but since the direction of movement is restricted by the inner wall of the reaction vessel, the stirring ball rotates in the reaction vessel and stirs the liquid to be stirred.

In a preferred embodiment of the present invention, the reaction disk is reciprocated at a high speed under a vibration condition of an amplitude of 0.8 to 3.0 mm and a frequency of 10 to 40 Hz in order to obtain efficient stirring. By setting the diameter of the stirring ball to half or less of the inner diameter of the reaction vessel and setting the specific gravity of the stirring ball to the liquid to be stirred to be 4 or more, suitable stirring without running out of the liquid from the reaction vessel is performed. Further, since the stirring balls are put into the respective reaction vessels on the reaction disk, no carryover occurs between the reaction solutions via the stirring balls.

When the present invention is practically applied to an automatic analyzer,
High photometric accuracy must be obtained. By forming a pair of smooth light projecting windows in a reaction container having a curved inner wall side surface, a stable photometric value can be obtained even if the position of the reaction container in the optical path position of the luminosity system is slightly shifted. The rotational movement of the stirring ball can also be suitably performed. By forming the stirrer with a ferromagnetic material and providing the magnet near the photometry position, it is possible to prevent the stirrer from obstructing the optical path during photometry.

Since the entire reaction disk is vibrated, the liquids in the plurality of reaction vessels on the reaction disk are stirred at the same time, and this stirring is performed each time a sample and reagent are added to a new reaction vessel. The reaction solution is frequently stirred during the period from to the measurement. When an insoluble reagent having a specific gravity different from that of the liquid is contained in the reaction vessel, the reaction is promoted by such repeated stirring.

〔Example〕

One embodiment of the present invention will be described with reference to FIGS.

A plurality of reaction vessels 2 are arranged on the circumference of a rotary disk-shaped reaction disk 1, and the reaction disk 1 is rotated by a driving mechanism 3. The drive mechanism 3 allows the reaction vessel 2 to rotate intermittently one pitch at a time or to make a short-cycle reciprocating movement.
The reaction disk 1 is reciprocated at a high speed with a small amplitude, and the liquid in the reaction container is stirred.

As shown in FIG. 3, a reaction ball 2 made of permalloy is previously placed in the reaction vessel 2 mounted on the reaction disk 1. The reaction vessel in FIG. 3 is for fluorescence photometry. Since the upper end of the reaction vessel 2 is sealed by the aluminum film 5, the stirring ball 4 does not jump out of the reaction vessel 2 during transportation. This reaction vessel 2 has a cylindrical shape with an inner diameter of 6.2 mm and a depth of 30 mm, has a smooth entrance window 24 on the bottom surface, and a smooth exit window on the side surface.
Has 25. The reaction vessel 2 is made of glass or acrylic resin which is a translucent material. When the reaction vessel 2 is set on the reaction disk 1, a hole 5a having a desired size is formed in the seal film 5 by a seal breaker device (not shown). Therefore, the dispensing operation of the sample and / or the reagent subsequently performed by the probe 15 of the dispensing mechanism 14 is not hindered by the seal film 5.

As shown in FIG. 1, a permanent magnet or electromagnet 7 is arranged near the photometry position of the photometer 19 inside the reaction thermostat 6.
Since the stirring ball 4 in the reaction vessel which has reached the photometry position is attracted to the side wall opposite to the emission window 25 by the magnet 7, the stirring ball 4 does not obstruct the passage of the light flux 22.

On the other hand, the rotating disk-shaped sample disk 8 and the rotating disk-shaped reagent disk 9 are arranged concentrically, and the sample disk 8 and the reagent disk 9 are simultaneously rotated by the central drive shaft 10. I do. Although the sample disk 8 is provided on the center side and the reagent disk 9 is provided on the outer peripheral side in the drawing, they may be provided in reverse. A plurality of sample containers 11 are placed on the sample disk 8.
Are arranged. On the reagent disk 9, a reagent container group 12 in which several types of reagent containers are grouped is arranged.

The reagent container 12 arranges a first reagent, a second reagent, and the like for a specific analysis item as a group. The reagent disk 9 and the sample disk 8 are rotated around a drive shaft 10 and the reagent container 12 is rotated.
The sample container 11 is rotated by one pitch or a designated number of pitches. In addition, the reagent container 12 and the sample container 11 are separately attached to the analysis object, and are detachably set. Further, the sample container 11 is separately arranged in the sample thermostat and the reagent container 12 is separately arranged in the reagent cooler 13 to maintain a predetermined temperature.

A pipetting mechanism 14 is provided for dispensing the above-described sample, standard substance, or reagent from the sample container 11 or the reagent container 12 to the reaction container 2. The pipetting mechanism 14 is provided with a probe 15 at the tip of a rotating arm 14a,
The sample or the reagent is sucked by the probe 15, and the probe 15 is rotated and discharged to the reaction container 2 at the sample and reagent dispensing position 16. At this time, the sample container 11 or the reagent container 12 to be dispensed is arranged on the movement locus of the probe 15 of the pipetting mechanism 14, and the sample disk 8 or the reagent disk 9 is rotated by the drive shaft 10 to move along the movement locus. To stop. Further, a probe cleaning device 17 is provided, and cleaning water is pumped into and out of the probe 15 to sufficiently clean the probe.

A predetermined amount of the sample is sucked by the probe 15 from the sample container 11 on the sample disk 8 by the pipetting mechanism 14 by the probe 15 and weighed, transferred to the reaction container 2 at a designated position on the reaction disk 1 and discharged. After dispensing, pipetting mechanism 14
The probe 15 is sufficiently washed by the washing device 17 to prevent contamination by carry-over of the sample solution. Next, the reaction disk 1 was moved by the high-speed reciprocating drive mechanism 3 at a frequency of 33 Hz and an amplitude of 1.2 mm.
After reciprocating for two seconds, it rotates so as to advance one pitch.

As shown in FIG. 1, the high-speed reciprocating drive mechanism 3 uses a stepping motor 3a as a power source and is connected to the rotating shaft 3c of the reaction disk 1 by a gear or a connecting belt 3b. Of course, the rotation axis of the step motor 3a and the rotation axis 3c of the reaction disk
Can be integrated, in which case neither a gear nor a connection belt is required. The operation of the stepping motor 3a is controlled by the central processing unit 18 and rotates in the forward and reverse directions by 5 pulses each for 30 msec, and repeats this for 3 sec. Reciprocate. Thereby, the reaction vessel also reciprocates at a high speed of about 33 Hz, and by using a reaction disk having a diameter of about 300 mm, an amplitude of about several mm is obtained depending on a gear ratio and the like. The high-speed reciprocating drive mechanism 3 is also used for rotating the reaction disk for step feed and moving the reaction container 2 to a target position.

On the other hand, the sample disk 8 is rotated to the next suction pipetting position. By repeating this operation sequentially, a required number of sample liquids are first transferred and dispensed into the reaction vessel 2. Next, the sample solution is similarly poured from the sample container 12 into the pipetting mechanism 14.
And dispenses to the reaction container 2 at the sample and reagent dispensing position 16.

Next, the reaction disk 1 is moved by the high-speed reciprocating drive mechanism 3 to 3
By reciprocating for 2 seconds, the reaction solution in the reaction vessel 2 is stirred and then transferred by one pitch rotation.

The reagents are sequentially transferred and dispensed from the first reagent in the reagent series in the reagent container group. In this way, the designated rotation is performed on the reaction disk 1, and the sample and the reagent are batch-dispensed into the reaction container 2. As a sample, a biological fluid such as serum, plasma, or urine is used. As the reagent, the same reagent as that usually used can be used.

At the sample and reagent dispensing position 16, the sample and the reagent sequentially dispensed into the reaction container 2 start a reaction in the reaction container 2. For example, the interval at which the reaction vessel is transferred by one pitch is 18
Assuming that the reciprocating drive time of the reaction disk 1 is 3 seconds, all the reaction vessels on the reaction disk 1 are 3 seconds every 18 seconds.
The reciprocating motion for a second is repeated. As a result, the reaction liquids in all the reaction vessels are agitated for 3 seconds every 18 seconds in the whole reaction process. When a coloring reagent is added to the reaction container at the reagent dispensing position 16, a color reaction proceeds.

The photometer 19 is a multi-wavelength simultaneous photometric type having a plurality of detectors, and is arranged so that the reaction vessel located at the photometry position 20 on the reaction disk 1 facing the reaction vessel 2 passes through the light flux 22 from the light source lamp 21. Is configured.

In FIG. 1, light from a light source lamp 21 is
The light is condensed by a and b, and is incident as excitation light from the incident window 24 on the bottom surface of the reaction vessel 2 into the reaction solution in the reaction vessel. The fluorescence emitted from the reaction solution is taken out from the emission window 25 of the reaction vessel, and the fluorescence intensity is detected by the photomultiplier 26 through the lens 23c. By the transfer operation of the reaction disk 1, the reaction vessels are successively positioned at the photometry position 20, and the fluorescence intensity based on each sample is measured by the photometer 19.
As for the output of the photometer 19, a signal of a currently required measurement wavelength is selected by a multiplexer, taken into the central processing unit 18 by the A / D converter 27, and stored in the RAM.

FIG. 4 is a flow chart showing a series of operations from the dispensing of the sample and the reagent to the end of the measurement, including a stirring operation by high-speed reciprocating motion.

The central processing unit 18 controls the entire apparatus including the mechanical system and performs all data processing such as density calculation, and uses a microcomputer.

The effect of stirring the reaction solution on the progress of the chemical reaction
Shown in the figure. When the same reagent for theophylline measurement as in Experimental Example 1 was reacted with the theophylline standard solution at 30 μg / ml, the first
The relationship between the total stirring time in the entire reaction process from the addition of the reagent to the photometry and the fluorescence intensity resulting from the progress of the reaction is shown. In FIG. 5, data A shows data when the reaction solution was stirred for 3 seconds each time the reaction vessel was transferred by one pitch using the automatic analyzer of this embodiment, and the sample and the reagent were mixed. The reaction solution is continuously and completely stirred in the entire reaction process from the start of the reaction to photometry. Data B corresponds to the case where a conventional automatic analyzer is used, but the reaction solution is stirred only once per reaction step.

As is clear from FIG. 5, the reaction was accelerated as the stirring of the reaction solution was performed more frequently (that is, the total stirring time was increased), and the fluorescence intensity generated as a result of the reaction was significantly increased. However, even if a more frequent stirring was attempted than the stirring condition (condition of data A) employed by the automatic analyzer of the present invention, the fluorescence intensity obtained as shown by data C in FIG. It was almost the same as A, and no further promotion of the reaction was observed. This indicated that Data A was the point at which the reaction proceeded most efficiently with frequent stirring. According to the above results, the stirring of the reaction solution in the reaction process has a great influence on the promotion of the reaction, and the reaction solution is continuously stirred in the entire reaction process as in the automatic analyzer of this example. Thus, it is clear that the progress of the reaction is remarkably accelerated.

In addition, when a component that is insoluble and has poor dispersibility is contained in the reaction solution, it is necessary to prevent sedimentation by frequent stirring to promote the reaction. The stirring method described above is useful.

Various materials such as an aluminum film, a polyethylene film, and a silicon film can be used as a sealing material when the reaction vessel 2 containing a stirrer in advance is used. A seal breaker is provided separately from the dispensing probe to easily break the seal 5 so that the seal 5 does not hinder the dispensing when dispensing the sample or the reagent by the dispensing probe 15. Prior to dispensing into the container, the seal 5 may be broken or a dispensing probe
You may break the seal at 15.

Glass and plastics can be used as the material of the reaction vessel 2. The strength of the container, the low adsorbability of the reaction reagent and the sample, the low cost, and the good light projection property are required especially when the reaction liquid is directly measured, and an acrylic resin can be suitably used.

Here, permalloy is used as the material of the stirrer 4, but any material having a specific gravity greater than 1 with respect to the solution to be stirred may be used as the stirrer. By changing the size of the stirrer according to the amount and viscosity of the solution to be stirred, the stirring effect can be improved. However, those that easily rust, such as iron, and those that cause a chemical reaction with a solution and adversely affect the original reaction, require a surface treatment such as plastic coating or plating on the stirrer. In the case of direct photometry, if a ferromagnetic material such as iron or permalloy is used, the light flux 22 can be easily avoided by the magnetic force of the magnet. In this case, regardless of whether the ferromagnetic material itself reacts or not, when a ferromagnetic material participates in the reaction, for example, in a reaction using an iron catalyst or the like, if residual magnetism remains in the stirrer 4,
It is conceivable that the ferromagnetic substance and the stirrer 4 in the reaction solution are adsorbed and adversely affect the reaction. In this case, it is necessary to use a material having a small residual magnetism as the stirrer 4. Permalloy is less likely to have residual magnetism, and is suitable for reactions in which residual magnetism becomes a problem. The shape of the stirrer is preferably substantially spherical.

Next, the effects of high-speed reciprocating motion conditions, the shape of the reaction vessel 2 and the shape of the stirrer on the stirring efficiency will be described with reference to FIGS. In FIG. 6, the vertical axis represents the amplitude of the high-speed reciprocating motion, and the horizontal axis represents the frequency.

In case of spherical stirrer (hereinafter referred to as stirrer ball), Fig. 6
When a sufficiently large high-speed reciprocating motion as shown in A, B and E is applied to the cylindrical reaction vessel 35, the stirring ball 4 revolves along the inner wall surface of the cylindrical vessel 35 as shown in FIG. According to such a revolving motion of the stirring ball 4, the stirring is completed within 3 seconds when the liquid depth is within 10 times the diameter of the stirring ball. This is because a swirl occurs in the solution due to the revolution of the stirring ball 4, and the same result as that of the vortex mixer or the magnetic stirrer can be obtained.

Even if the reaction vessel has the same high-speed reciprocating motion, if the reaction vessel has the shape of a square pillar, if the bottom surface is flat, the diameter of the stirring ball 4 is 2-3
It can only be stirred up to twice the height (FIG. 7B). However,
Under the same conditions, a high-speed reciprocating motion in the diagonal direction of the square prism would result in a seventh
As shown in FIG. C, the stirring ball 4 moves two-dimensionally on the bottom surface of the rectangular column container 36, and when the liquid depth is within 10 times the diameter of the stirring ball 4, the stirring is completed in about 5 seconds.

When a reciprocating motion having a frequency and an amplitude in the range of FIG. 6C is applied to a reaction vessel having a flat bottom, the revolving motion of the stirring ball 4 in the cylindrical vessel 35 no longer occurs as shown in FIG. 7D. Therefore, when the liquid depth is within 10 times the diameter of the stirring ball 4, a stirring time of 3 to 20 seconds is required. FIG. 7E
As shown in Fig. 7, when the reciprocating reciprocation is performed in the side direction of the rectangular column container 36, the stirring can be performed only up to about twice the diameter of the stirring ball 4. However, as shown in FIG.
Even when 36 is reciprocated at high speed in the diagonal direction, the same stirring efficiency as that of the cylindrical container can be obtained.

Even if a high-speed reciprocating motion having a frequency and an amplitude in the range of D shown in FIG.
Can only be stirred up to about twice the height of the diameter. However, when a step having a height about the radius of the stirring ball 4 is provided on the inner circumference of the bottom surface as shown in FIGS. 7G and 7H, the horizontal movement of the stirring ball 4 is added to the vertical movement, thereby improving the stirring efficiency. As an alternative to this step, a depression (FIGS. 7I and 7J), a step that traverses the bottom surface (FIGS. 7K and 7L), and other bottom shapes can be considered. Also in this case, the stirring efficiency of the cylindrical container 35 (G, I, K in FIG. 7) is higher than that of the rectangular column container 36 (H, J, L in FIG. 7). This is because when the collision angle between the stirring ball 4 and the reaction vessel is projected on the bottom surface, the angle is always 90 ° in the case of the rectangular column vessel 36, while the angle is variously 0 ° to 90 ° in the case of the cylindrical vessel 35. This is because the moving range of the stirring ball 4 is widened. In this case as well, if the rectangular column container 36 is reciprocated at high speed in the diagonal direction, the stirring efficiency becomes substantially the same as that of the cylindrical container 35.

When a bar-shaped stir bar 37 is used as shown in FIGS.
Since a wide range of the solution can be moved at the same time, the solution can be stirred. When the rod-shaped stirrer 37 is used, the stirring ball 4
As in the case where is used, the moving range of the rod-shaped stirrer 37 is widened and the stirring efficiency is improved, but it is not preferable in terms of photometry.

In the case of direct photometry, if the stirring ball 4 is moved up and down by providing a step or a depression on the bottom surface as described above, or if a rod-shaped stirrer 37 is used, the light-transmitting surface on the side surface of the reaction vessel 2 may be used. It is unsuitable because it can cause damage. Further considering the stirring efficiency, when a cylindrical container is used, A in FIG.
And the ranges of the frequency and amplitude of B are suitable for stirring. However, in the range of A, the high-speed reciprocating motion is too intense, and the solution may scatter from the reaction vessel. Therefore, the range B in FIG. 6 is practically suitable.

When high-speed reciprocating agitation is actually applied to an automatic analyzer, reciprocating with an amplitude larger than one step, for example, when direct photometry is performed while reciprocating at high speed, the reaction vessel deviates from the luminous flux, making measurement difficult. And the reaction vessel 2 containing the ferromagnetic stirrer 4 is a magnet 7
When the reaction vessel 2 is located next to the photometric unit in which is disposed, the reaction vessel 2 reciprocates between the position of the magnet 7 and a position where the magnet 7 is not present, thereby causing problems such as bubbling and scattering of the solution. Therefore, it is desirable that the amplitude is smaller than one step.

As is clear from FIG. 6, as the frequency is increased, B
The range of the amplitude of the signal becomes narrow. This is because the variation in the amplitude in the high-speed reciprocating motion of the reaction vessel caused by the variation in the meshing of the gears in the high-speed reciprocating drive mechanism 3 of the reaction disk, etc.
If the distance is several tenths of a millimeter, the vibration condition of the high-speed reciprocating motion shifts from B, which is an appropriate range, to A, C, or D, which is an inappropriate range, and stable stirring cannot be obtained.

Taking these facts into consideration, it has been found that the range of E in FIG. 6 is suitable as the high-speed reciprocating condition of the reaction vessel to be applied to the automatic analyzer. That is, an amplitude of 0.8 to 3.0 mm and a frequency of 10 to 40 Hz are appropriate.

FIG. 8 shows the relationship between the liquid depth and the specific gravity of the stirring ball (hereinafter referred to as the specific gravity with respect to the solution) required for stirring the solution at the liquid depth for 3 seconds. The vertical axis shows the specific gravity of the stirring ball to the solution to be stirred, and the horizontal axis shows the ratio of the liquid depth to the diameter of the stirring ball.

The specific gravity of the stirrer material with respect to the solution to be stirred, which is necessary to perform sufficient stirring with the stirring time of about 3 seconds, increases as the amount of the solution to be stirred increases. In the case of the stirring ball 4 shown in FIG. 1, when the liquid depth is about the diameter of the stirring ball 4, the stirring ball 4 needs a specific gravity to solution of about 1.5. To stir in seconds, a stirring ball having a specific gravity to solution of about 4 is required.

Further, even if the specific gravity of the stirring ball 4 with respect to the solution is set to 4 or more,
The stirring efficiency hardly changes. Therefore, not only the stirring by the stirring ball 4 but also the stirring of the solution by reciprocating the reaction vessel 2 at a high speed generally requires the stirrer 4 having a specific gravity to the solution of 1.5 or more. A stirrer having a solution specific gravity is suitable.

The upper limit of the specific gravity to solution is about 20 in practical use because most inexpensive substances such as iron, copper, and tungsten have a density within 20 g / cm ³ . Therefore, it can be seen that the range of the specific gravity to solution suitable for practical use as the stirrer 4 is 4 to 20.

It has been found that the relationship between the radius of the stirring ball and the radius in the cylindrical container that can be stirred using the ball is represented by the following equation.

D ≦ 4 (A ₂ + d), D ≧ 1.1d (d <10) D ≧ d + 1 (d ≧ 10) where A ₂ : Both amplitudes (twice the amplitude) (mm), d: Stirring ball diameter ( mm), D: Diameter of cylindrical vessel (mm) Considering that the size of the reaction vessel applied to an automatic analyzer is generally 30 mm or less, the range where the stirring efficiency is excellent is the range of both amplitudes A ₂ Is 7.5 mm or more, the range of 1.48d ≦ D ≦ 4.4d (A ₂ ≧ 7.5), and when both amplitudes A ₂ are 7.5 mm or less, (0.909A ₂ , 4A ₂ ), (2.73A ₂ , 4A ₂ ), the interior of the triangle formed by connecting the three points (0,0) and (0.909A ₂ , 4A ₂ ), (2.73A ₂ , 4A ₂ ), (22.2−0.25A, 30), ( 12.5−0.75A ₂ , 30) and ((0.909A ₂ , 4A ₂ )) were found to be trapezoidal.

FIG. 9 shows D and d that can be stirred when both amplitudes A ₂ are 2 mm.
Is shown by a graph. The vertical axis is the diameter D inside the cylindrical container
In (mm), the horizontal axis is the stirring ball diameter d (mm). The range A indicates a range in which stirring is possible, and the range B indicates a range particularly suitable for an automatic analyzer.

FIG. 11 shows a configuration of an embodiment in the case where the transmitted light characteristic of the reaction solution is measured using the reaction vessel 2a shown in FIG. Components having the same functions as those of the embodiment of FIG. 1 are denoted by the same reference numerals. An entrance window 24a and an exit window 25a which are parallel to each other are formed in the cylindrical reaction vessel 2a shown in FIG. When measuring the transmitted light, the stirrer 4 sinks to the bottom of the reaction vessel 4 as shown in FIG. 11, so that the light flux position is set above the stirrer to prevent shading by the stirrer. can do. In this case, the material of the stirring ball 4 is not limited to a ferromagnetic material, but may be a metal such as aluminum or copper, a non-metal such as glass, or a magnet.

FIG. 13 shows various shapes of the reaction vessel. A plurality of flat transmission windows are formed on the side surface of the cylindrical container. As shown in FIG. 13A, a substantially cylindrical container having two planar light transmission windows facing the side surface of the cylindrical reaction container 2 can be used for light absorption measurement.
One in which two light transmission windows form an angle of 90 ° with each other as shown in FIG. 13B can be used for fluorescence measurement, and three planar light transmission windows can be used with a 90 ° angle as shown in FIG. 13C. Those arranged at intervals can be used for simultaneous measurement of light absorption and fluorescence.

Experimental Example 1 An example of analyzing theophylline using the automatic analyzer shown in Example 1 of FIG. 1 will be described.

The reagent used was Ames TDM ^™ Theophylline ^Kit (manufactured by Miles Sankyo Co., Ltd.).

To the sample disk 8, the theophylline standard solution (0, 10, 20, 30, and 40 μg / ml) was placed in the sample container 11 and set. The reagent for theophylline measurement (first
Reagents: β-galactosidase and anti-theophylline antibody, Second reagent: fluorescently labeled theophylline (β-galactosyl)
-Umbelliferone-theophylline)).

After mixing 50 µ of the sample with 250 µ of the first reagent and reacting for 36 minutes, 50 µ of the second reagent was added, and 5 minutes later, measurement was performed at an excitation wavelength of 400 nm and a fluorescence wavelength of 450 nm. FIG. 10 shows a standard curve prepared by plotting the measured theophylline concentration of the standard solution on the horizontal axis and the fluorescence intensity of the measured standard solution on the vertical axis.

〔The invention's effect〕

As described above, according to the present invention, it is possible to efficiently stir the liquid in the reaction vessel with a simple configuration, and it is not necessary to share a stirrer, so that stirring without carryover can be performed. .

[Brief description of the drawings]

FIG. 1 is a schematic diagram showing a main part of the embodiment of FIG.
FIG. 1 is a schematic plan view for explaining one embodiment of the present invention, FIG. 3 is a partially cutaway sectional view of a reaction container for fluorescence photometry,
FIG. 4 is a flow chart showing the measuring operation process of the embodiment of FIG. 2, FIG. 5 is a graph showing the relationship between the stirring time and the fluorescence intensity, FIG.
The figure shows the movement of the stirrer under the conditions of FIG. 6, FIG. 8 is a graph showing the relationship between the liquid depth and the amount of liquid that can be stirred with respect to the diameter of the stirring ball, and FIG. 9 is the case where both amplitudes are 2 mm. FIG. 10 is a graph showing the relationship between the inside diameter of a stirrable cylindrical reaction vessel and the diameter of a stirring ball, FIG. 10 is a view showing a standard curve of theophylline measured using the apparatus of the embodiment of FIG. 2, and FIG. FIG. 12 is a schematic configuration diagram showing a main part of the embodiment of FIG. 12, FIG. 12 is a diagram showing the configuration of a light absorption direct photometric
FIG. 13 is a schematic view showing various embodiments of the reaction vessel. DESCRIPTION OF SYMBOLS 1 ... Reaction disk, 2 ... Reaction container, 3 ... Drive mechanism, 4 ... Stirring ball or stirrer. 5 …… Seal, 8…
... Sample disk, 9 ... Reagent disk, 14 ... Piping mechanism, 15 ... Probe, 18 ... Central processing unit, 19
… Photometer, 20 photometry position, 24 entrance window, 25 exit window.

 ──────────────────────────────────────────────────続 き Continuation of the front page (72) Inventor Hiroshi Umezu 882 Ma, Katsuta-shi, Ibaraki Pref. Naka Plant of Hitachi Ltd. (56) References JP-A-62-133354 (JP, A) JP-A-58 -131567 (JP, A) Fully open Showa 60-139270 (JP, U)

Claims (7)

(57) [Claims] 1. A plurality of reaction vessels each containing a stirrer made of a ferromagnetic material, a reaction disk on which the plurality of reaction vessels are arranged, and an intermittent transfer motion and a short-period reciprocating motion on the reaction disk. A driving device for providing vibration;
A device for supplying a sample and a reagent to the reaction container, a photometer for irradiating the reaction container with light and measuring the reaction liquid in the reaction container, and a photometer disposed near the photometry position of the photometer; An automatic analyzer comprising: a magnet for attracting the stirrer to the reaction vessel wall so that the stirrer in the reaction vessel positioned at the position does not obstruct the optical path of the photometer. 2. A reaction container containing a stirring ball is arranged on a reaction disk, and the reaction disk is reciprocated at a high speed in an arc shape to vibrate. The vibration causes the stirring ball in the reaction container to rotate. An automatic analyzer characterized by stirring a liquid in a reaction vessel. 3. The apparatus according to claim 2, wherein said vibration has an amplitude of 0.8 to 3.0 mm and a frequency of 10 to 10 mm.
An automatic analyzer characterized by a frequency of up to 40 Hz. 4. The automatic analyzer according to claim 2, wherein the specific gravity of the stirring ball with respect to the liquid in the reaction vessel is 4 or more. 5. The apparatus according to claim 2, wherein the inner diameter of the reaction vessel is two times the diameter of the stirring ball.
An automatic analyzer characterized by being at least twice as large. 6. A plurality of reaction vessels containing a stirrer are arranged on a reaction disk, and a sample and a reagent are added to a corresponding reaction vessel at a predetermined position while the reaction disk is stopped. The liquid in the plurality of reaction vessels is agitated by vibrating the reaction disk by continuously reciprocating in a short cycle, and the reaction to which the sample and the reagent are added is performed by advancing the reaction disk. An automatic analyzer configured to advance the container to the photometric position. 7. A reaction vessel having at least a portion of the inner wall side surface curved and having a pair of smooth translucent windows, wherein a substantially spherical stirrer is housed inside, and a stirrer escape is provided at an upper end. A reaction vessel equipped with an outflow prevention membrane.