JPH0499961A - Injecting apparatus for test solution into test container - Google Patents

Abstract

PURPOSE:To obtain a simple apparatus capable of injecting a test solution accurately and rapidly in low cost by providing a suction nozzle whose lower end suction port rises and falls in a test container, a test solution supply means and a drive control mechanism for them. CONSTITUTION:After a test container 12 is filled with a test solution 66 in an amount more than a set amount by a predetermined amount, the lower end suction port of a suction nozzle 24 is allowed to fall in the container 12 by a nozzle driving mechanism 54 so as to reach the vicinity of the surface of the solution and the liquid 66 is sucked in the vicinity of the surface thereof along with air by a vacuum pump 56 and the liquid 66 in the container 12 is gradually discharged and reduced with the falling operation of the nozzle 24 and, when the nozzle 24 reaches the position corresponding to the set amount, the vacuum pump is stopped to stop suction and the set amount of the solution 66 is left in the container 12. By this method, accurate and rapid injection can be simply carried in low cost.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a dissolution test device that measures the degree of dissolution of formulation components when a solid formulation such as a tablet, granule, or capsule is immersed in a solvent. The present invention relates to a test liquid injection device that allows a set amount of water or chemical liquid to be injected into a test container.

[Conventional technology]

For dissolution testing of solid preparations such as tablets, granules, and capsules,
In recent years, it has become important as a method for evaluating the quality of pharmaceutical preparations. This dissolution test examines the dissolution rate of herbal medicines when solid preparations are immersed in various solvents.A predetermined amount of solid preparations is poured into a test container and placed into various solvents maintained at a temperature of 37°C. This is done by adding a portion of the solution several times over time, and sequentially measuring the absorbance of each sample using spectrophotometry to record changes over time in the amount of the crude drug eluted. Furthermore, when simultaneously measuring multiple components in a preparation, a sample liquid is fractionated and subjected to liquid chromatography analysis.

In this elution test method, the radius is 50 to 52.5 m.
It has a semicircular inner bottom surface with a wide opening at the top end surface, and has a capacity of 1. A OOOmfl glass container is used, and a set amount of test liquid (solvent) is injected into this test container for every 100 mfl in the range of 500 to 900 mQ, and the solid preparation is poured into the test liquid and dissolved. Ru. Here, in order to inject the test liquid into the test container, conventionally, the test liquid is weighed manually using a measuring cylinder or volumetric flask, and the weighed test liquid is transferred from the measuring cylinder or volumetric flask to the test container. I was trying to move it.

Also, for example, Japanese Patent Publication No. 63-38097, Japanese Patent Publication No. 63-38097,
As disclosed in JP-A-3-38098, JP-A-57-4, JP-A-4853, etc., a test container and a spare container for storing the test liquid are placed side by side, and at the beginning of the dissolution test, By operating the pump, a predetermined amount of the test liquid is injected from the reserve container into the test container through an injection container disposed between the reserve container and the test container. Alternatively, JP-A-63-196859 discloses that by operating a solenoid valve, a test liquid is introduced into a test container from a test liquid warmer that heats the test liquid to an appropriate temperature and stores it. Additionally, a fully automatic dissolution test device is disclosed in which a liquid level sensor senses the liquid level of a test liquid and automatically injects a predetermined amount of the test liquid into a test container.

[Problem to be solved by the invention]

However, the method of manually weighing the test liquid into test containers using a graduated cylinder or volumetric flask requires a lot of effort and time, especially when the number of test containers increases, such as six. The work becomes troublesome, and weighing errors may occur.

In addition, as disclosed in Japanese Patent Application Laid-open No. 63-38097, etc., a method in which a pump is operated to send the test liquid from a preliminary container to a test container, and a predetermined amount of test liquid is injected into the test container does not require a syringe. The test liquid is pumped into the test container by using an expensive pump that can control the amount of liquid sent with high precision, such as a type pump, and by appropriately controlling the number of input pulses to the pulse motor that drives the pump. It is necessary to program the injection amount so that it is exactly as set.

For this reason, there are problems in that the device configuration becomes complicated, costs increase, and programming work is also dangerous.

On the other hand, as disclosed in Japanese Unexamined Patent Publication No. 63-196859, the method of adjusting the amount of test liquid injected into a test container to a constant amount by a combination of a solenoid valve and a liquid level sensor is not practical. In order to perform accurate liquid volume control, a special liquid level sensor with high detection accuracy is required, and in systems with multiple test containers arranged side by side, a liquid level sensor and a solenoid valve are installed for each test container. It is necessary to provide a drive control mechanism for this purpose. In addition, when detecting the liquid level with a liquid level sensor, the liquid level ripples as the test liquid is poured into the test container, making it difficult to accurately detect the liquid level. In order to avoid ripples on the surface, the test liquid can be poured into the test container gently at a low flow rate, but this poses a problem in that the injection operation of the test liquid takes time.

This invention was made in view of the above-mentioned circumstances, and when automating the operation of injecting test liquid into test containers, it is difficult to use expensive pumps and complicated drive controls as in the past. The technical challenge is to automate this process without requiring a lJ control mechanism or using a solenoid valve or liquid level sensor to adjust the injection amount, and with this, we will set up a test container. The purpose of the present invention is to provide a device for injecting a test liquid into a test container, which can accurately and quickly inject the correct amount of test liquid, has a relatively simple configuration, and is not very expensive. do.

[Means to solve the problem]

As a means for achieving the above-mentioned object, the present invention provides a test liquid injection means for supplying a predetermined amount of test liquid to a test container that is larger than a set amount, and a lower end suction port that enters into the test container and moves up and down within the test container. A freely supported suction nozzle, a nozzle rotation mechanism that moves the suction nozzle up and down, a vacuum suction means connected to the suction nozzle through a flow path, and controls the operation of the nozzle movable mechanism and the vacuum suction means. The gist of this invention is to configure a test liquid injection device from a control means to a test container. The vacuum suction 1 means can suck the test liquid from near the liquid surface along with air through the lower end suction port as the suction 1 nozzle descends;
The control means controls the nozzle disengagement mechanism to lower the suction nozzle to a position corresponding to the set amount of test liquid and then stop it.

The vacuum suction means includes an airtightly sealed waste liquid tank;
A suction pipe that communicates the waste liquid tank with the suction nozzle, a suction control valve inserted in the middle of the suction pipe, a vacuum pump that is connected to the waste liquid tank via a vacuum pipe, and a vacuum pump that communicates with the waste liquid tank via the vacuum pipe. It can be configured to include a pressure release valve attached to the waste liquid tank for opening the inside of the waste liquid tank to the atmosphere, and a discharge valve attached to the waste liquid tank for discharging the test liquid remaining in the waste liquid tank. Further, a configuration may also be adopted in which a cleaning liquid supply means for supplying a predetermined amount of cleaning liquid to the test container is provided.

[For production]

In the apparatus for injecting a test liquid into a test container having the above configuration, first, the test liquid injecting means injects a predetermined amount of the test liquid into the test container, which is larger than the set amount, and fills the test container with the test liquid. Subsequently, the nozzle sliding mechanism is controlled by the control means, and the suction nozzle is lowered by the nozzle sliding mechanism. When the lower end suction port of the suction nozzle enters into the test container and the lower end suction port descends to near the liquid level of the test liquid, the vacuum suction force of the vacuum suction means causes the suction nozzle connected to it to enter the test container near the liquid level. The test liquid is sucked in together with air from the lower suction port. Then, as the suction nozzle moves downward, the test liquid is gradually discharged from the test container through the suction nozzle, and the test liquid in the test container gradually decreases. Finally, when the suction nozzle descends to a position corresponding to the set amount of test liquid, the nozzle movement mechanism is controlled by the control means to stop the downward movement of the suction nozzle. At this point, a set amount of test liquid will remain in the test container.

In this way, this test liquid injection device first fills the test container with approximately the same amount of test liquid that is larger than the set amount, and then drains the test liquid in excess of the set amount from the test container.
Since the set amount of test liquid determined by the downward stop position of the suction nozzle ultimately remains in the test container, very high precision is not required for controlling the amount of liquid fed by the test liquid injection means. In addition, there is no need for a liquid level sensor or solenoid valve to control the liquid volume, and even if multiple test containers are installed in parallel in the dissolution test device, multiple suction nozzles installed for each test container can be used. If the suction nozzles are integrally connected and the plurality of suction nozzles are moved up and down integrally by a common nozzle movement mechanism, there is no need to control the liquid volume for each test container. In this test liquid injection device, the test liquid is injected into the test container at once by the test liquid injection means, and then the suction nozzle is lowered at an appropriate speed to fill the set amount of test liquid into the test container. Since the liquid is injected, the test liquid injection operation can be completed in a short time.

Incidentally, when a cleaning liquid supply means for supplying a predetermined amount of cleaning liquid to the test container is provided, the cleaning operation of the test container can also be performed automatically.

〔Example〕

Hereinafter, preferred embodiments of the present invention will be described with reference to the drawings.

FIG. 1 shows one embodiment of the present invention and is a schematic diagram of a test liquid injection device into a test container, which constitutes a part of a dissolution test device, and FIG. 2 shows an elution device of the dissolution test device. FIG. Incidentally, in FIG. 2, the drive mechanism of the paddle (stirring blade) and the like, which are not directly related to the present invention, are not shown.

First, the configuration of the elution device section will be explained with reference to FIG. The elution device section is equipped with a constant temperature water tank 10 made of transparent glass filled with constant temperature water whose temperature is controlled to 37°C, and in this constant temperature water bath 10, six round-bottomed test containers are placed in the constant temperature water tank 10. 12 are respectively attached by fitting almost the entire body of the test container 12 through an oval hole formed in the upper wall surface covering the upper surface of the constant temperature water tank 10 and engaging the flange portion with the peripheral edge of the circular hole. There is.

The upper end opening surface of each test container 12 is closed by a lid 14, respectively. A groove-shaped hole 16 is formed in the lid 14, which is cut from its periphery to a position corresponding to the center position of the upper end opening surface of each test container 12. and,
Shafts 22 (only a portion of which is shown) having stirring blades 20 integrally formed at their lower ends are suspended through each groove-shaped hole 16 of the lid 14, and the upper end of each shaft 22 is connected to a rotating shaft (not shown). connected to a drive mechanism. In addition, the lid 14
A suction nozzle 24 is suspended through each of the groove-like holes 16 . The lid 14 further includes a sampling hole 26.
is formed, the sampling nozzle 28 is lowered through the sampling hole 26, and the sampling nozzle 28
This allows a portion of the eluate in the test container 12 to be collected and sent to an analysis device (not shown) such as a spectrophotometer. Further, a test liquid injection nozzle 30 and a pair of cleaning liquid supply nozzles 32, 32 are arranged at the upper end opening of the test container 12 so as to face into each test container 2.

The six suction nozzles 24 are each fixed to one connecting plate 34 at the upper end, so that the six suction nozzles 24 move up and down as one. Further, the connecting plate 34 includes a U-shaped support plate 3, as shown in FIG.
6 and is supported. A nut member 38 and a pair of bearing members 40, 40 are integrally fixed to the support plate 36.

The nuts 1 to 38 are screwed onto a threaded rod 42 held in a vertical position, and a pair of bearing members 40
．． 40 denotes each guide rod 4 held parallel to the tension rod 42.
4.44, respectively, and are slidably engaged with screw studs 4 and 44.
By driving a drive motor 46 with a rotating shaft connected to the lower end of the threaded rod 42 in the forward and reverse directions, the support plate 36 moves vertically while being guided by a pair of guide rods 44 and 44. Accordingly, the six suction bow nozzles 24 fixed to the connecting plate 34 are configured to move up and down at the same time. In addition, in FIG. 3, the guide shaft 44 is attached to the device fixing part
The parts that fix the are omitted from illustration.
Also, stirring blades, constant temperature water tanks, and their lids are not shown.
The configuration of the nozzle drive mechanism is made easy to understand.

Next, based on FIG. 1, the structure of the test liquid injection device other than the above will be explained. The suction bow nozzle 24 communicates with the internal space of the hermetically sealed waste liquid tank 50 via a suction pipe 48 connected thereto.
A suction control valve 52 is inserted in the middle. The waste liquid tank 50 is connected to a vacuum pump 56 via a vacuum piping 54.
is connected to. Further, the waste liquid tank 50 is provided with a pressure control valve 58 that opens the inside of the waste liquid tank 50 to the atmosphere, and is also provided with a drain pipe 60 that drains the liquid remaining in the waste liquid tank 50. A discharge valve 62 is provided in the drain pipe 60.

The test liquid injection nozzle 30 is connected to a test liquid tank 68 in which a test liquid 66 is stored via an injection pipe 64 connected thereto, and an injection pump 70 and an injection control device are connected to the injection pipe 64 in the middle of the injection pipe 64. A valve 72 is inserted in each case. The temperature of the test liquid 66 in the test liquid tank 68 is approximately 37°C.
is kept warm.

Further, the cleaning liquid supply nozzle 32 is connected to a cleaning liquid tank 78 in which a cleaning liquid 76 is stored through a liquid supply pipe 74 connected thereto, and a liquid supply pump 80 and a liquid supply pump 80 are disposed in the middle of the liquid supply distribution v74. A liquid control valve 82 is inserted in each. Then, it controls the nozzle drive mechanism 84 that moves the suction nozzle 24 downward by 2", and also controls each pump 56.7.
0.80 drive and stop, and various control valves 52.58
．． Control device for controlling the opening and closing of 62.72.82 (
A microcomputer 86 is provided. In addition, 88.90 in the figure is a liquid level sensor arranged inside the waste liquid tank 50.

Next, the operation of the test liquid injection device configured as described above will be explained based on FIG. 4.

In FIG. 4, the lid of the test container 12 and the like are not shown.

First, as shown in FIG. 4(a), with the suction nozzle 24 waiting in the upper position, the injection pump 70 is driven by a control signal from the control device 86, and the injection control valve 72 is opened. , the test liquid 66 is sent from the test liquid tank 68 to the test container 12 through the injection pipe 64, and the test liquid 66 is discharged from the test liquid injection nozzle 30 into the test container 12, as shown in FIG. 4(b). After injecting the test liquid 66 into the test container 12 in an amount that is about 50 mQ larger than the amount input and set in advance into the control device 86 using the keyboard, for example, 600 mu, the injection pump 70
and closes the injection control valve 72. next,
After driving the vacuum pump 56 and opening the suction control valve 52, the suction nozzle 24 is lowered at high speed by the nozzle dust movement mechanism 84, and the lower end suction port 92 of the suction nozzle 24 enters the test container 12. As shown in FIG. 4(c), when the lower end suction port 92 of the suction nozzle 24 descends to near the liquid level of the test liquid 66, the descending speed of the suction nozzle 24 is slowed down. At this time, the test liquid 66 near the liquid level is sucked into the suction nozzle 24 along with air from the lower end suction port 92 by the vacuum suction force of the vacuum pump 56, and subsequently, following the downward movement of the suction nozzle 24, it is drawn from the inside of the test container 12. Test liquid 6
6 through the suction nostle 24, e.g. 10 m f),
It is discharged at a speed of about / s e C, and the test container] 2
The amount of test liquid 66 in the container gradually approaches the set amount. The test liquid and air sucked into the suction nozzle 24 flow into the waste liquid tank 50 through the suction piping 48, and the air is exhausted through the vacuum piping 54 and the vacuum pump 56. continues to accumulate in the waste liquid tank 50.

Then, as shown in FIG. 4(d), when the lower end suction port 92 of the suction nozzle 24 descends to a position corresponding to the set amount, a signal from the control device 86 causes the nozzle m section movement mechanism 8 to move downward.
4 is controlled to stop the downward movement of the suction nozzle 24, and then the suction nozzle 24 is raised to return to the original two-way position shown in FIG. 4(e).

In this way, the set amount of test liquid 66 determined by the downward stop position of suction nozzle 24 ultimately remains in test container 12, and the test liquid injection operation is completed. And finally,
The test liquid accumulated in the waste liquid tank 50 can be disposed of through the drain pipe 60 by opening the pressure control valve 58 to bring the inside of the waste liquid tank 50 to atmospheric pressure, and then opening the discharge valve 62, or discarded for reuse. provide

The above-mentioned liquid volume adjustment operation shown in FIGS. 4(b) to 4(e) is performed by each suction nozzle 24 operating integrally for the six (in some cases, three) test containers 12. done at the same time. FIG. 5 shows a flowchart 1 of the above series of test liquid injection operations.

The configuration and operation of the device for injecting a test liquid into a test container have been described above, and according to this embodiment, it is also possible to automatically perform the cleaning operation of the test container. The cleaning operation of the test container will be explained based on FIG.

First, as shown in FIG. 6(a), with the suction nozzle 24 on standby at the upper position, the control device 86 drives the liquid feeding pump 80 and opens the liquid feeding control 82 to open the cleaning liquid tank 78. The cleaning liquid 76 is sent to the test container 12 through the liquid supply pipe 74, and the cleaning liquid 76 is injected into the test container 12 from the cleaning liquid supply nozzle 32 in a conical shape. At this point, the cleaning liquid 76 is sprayed onto the inner wall surface of the test container 12, flows down while wetting the entire surface of the inner wall, and accumulates on the inner bottom surface of the test container 12. Then, as shown in FIG. 6(b), when the stirring blade 20 is completely immersed in the cleaning liquid 76, the liquid feeding pump 80 is stopped in response to a signal from the control device 86, and the liquid feeding pump 80 is stopped. Control valve 82 is closed and supply of cleaning liquid 76 is stopped.

Next, after driving the vacuum pump 56 and opening the suction control valve 52, the nozzle drive mechanism 84 moves the suction nozzle 24 so that its lower end suction port 92 enters into the test container 12 and near the inner bottom surface of the test container 12. It is lowered at a constant speed until it reaches , and then stopped. During the descending process of the suction nozzle 24, as shown in FIG. 6(c), the cleaning liquid 76 is sucked together with air into the suction nozzle 24 through the lower end suction port 92 of the suction nozzle 24 by the vacuum suction force of the vacuum pump 56. As shown in FIG. 6(d), the cleaning liquid is completely drained from the test container 12. At this time, the cleaning liquid and air sucked into the suction nozzle 24 flow into the waste liquid tank 50 through the suction piping 48, the air is exhausted through the vacuum piping 54, and the cleaning liquid is stored in the waste liquid tank 50. It will be done. Finally, the suction nozzle 24 rises and returns to the original upper position shown in FIG. 6(e), completing one cleaning operation. Then, if necessary, the above series of cleaning operations is repeated several times. The cleaning liquid accumulated in the waste liquid tank 50 is
After the pressure control valve 58 is opened to bring the inside of the waste liquid tank 5o to atmospheric pressure, the discharge valve 62 is opened and the waste liquid is discharged through the drain pipe 60.

Although the device for injecting a test liquid into a test container according to the present invention has the above-described configuration, the scope of the present invention is not limited by the contents of the above description and drawings, and may be modified without departing from the gist. Various modifications may be included. That is, the configurations of the test liquid injection means, nozzle drive mechanism, vacuum suction means, etc. are not limited to those of the above embodiments.

[Effects of the Invention] Since the present invention is configured and operates as described above, it is possible to automatically inject a set amount of test liquid into a test container accurately and quickly, and the device configuration is superior to that of other devices. It has been possible to provide a device for injecting a test liquid into a test container that is simple, has a control mechanism that is not very complicated, does not have a very high cost, and is suitable for use in a dissolution test device or the like.

[Brief explanation of the drawing]

FIG. 1 is a schematic configuration diagram of a device for injecting a test liquid into a test container according to an embodiment of the present invention, FIG. The figure is a perspective view showing an example of the configuration of the nozzle drive mechanism, FIG. 4 is a vertical side view for explaining a series of operations in this test liquid injection device, and FIG. 5 is a series of test liquid injection operations. FIG. 6 is a longitudinal sectional side view for explaining the operation of cleaning the test container by the apparatus of the above embodiment. DESCRIPTION OF SYMBOLS 12... Test container, 30... Test liquid injection nozzle, 34... Connecting plate, 38... Nut member, 42... Screw head, 46... Drive motor, 50... Waste liquid tank , 54... Vacuum piping, 58... Pressure control valve, 62... Discharge valve, 66... Test liquid, 70... Injection pump, 74... Liquid feeding pipe, 78... Cleaning liquid tank , 82...Liquid feeding control valve, 86...Control device, 24...Suction nozzle, 32...Cleaning liquid supply nozzle, 36...Support plate, 40...Bearing member, 44...Guide Rod, 48... Suction pipe, 52... Suction control valve, 56... Vacuum pump, 60... Drain pipe, 64... Injection pipe, 68... Test liquid tank, 72... Injection control valve, 76...Cleaning liquid, 80...Liquid feeding pump, 84...Nozzle drive mechanism, 92...Lower end suction port. (a) (b) (e) (C)

Claims (1)

[Scope of Claims] 1. A test liquid injection means for injecting a predetermined amount of test liquid into the test container, and a suction device whose lower end suction port enters the test container and is supported so as to be able to rise and fall freely within the test container. a nozzle and
a nozzle drive mechanism that moves the suction nozzle up and down; a vacuum suction means connected to the suction nozzle through a flow path and sucking the test liquid from near the liquid surface together with air through the lower end suction port as the suction nozzle descends; A device for injecting a test liquid into a test container, comprising a control means for controlling the nozzle drive mechanism to lower the suction nozzle to a position corresponding to a set amount of the test liquid and stopping the suction nozzle, and a control means for controlling the operation of the vacuum suction means. . 2. The vacuum suction means includes an airtightly sealed waste liquid tank;
A suction pipe that communicates the waste liquid tank with the suction nozzle, a suction control valve inserted in the middle of the suction pipe, a vacuum pump that is connected to the waste liquid tank via a vacuum pipe, and a vacuum pump that communicates with the waste liquid tank via the vacuum pipe. 2. The test container according to claim 1, further comprising: a pressure release valve attached to the waste liquid tank for opening the inside of the waste liquid tank to the atmosphere; and a discharge valve attached to the waste liquid tank for discharging the test liquid remaining in the waste liquid tank. test liquid injection device. 3. The apparatus for injecting a test liquid into a test container according to claim 1 or 2, further comprising a cleaning liquid supply means for supplying a predetermined amount of cleaning liquid to the test container.