JP3007394B2 - Device for injecting test liquid into test container - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a dissolution test apparatus for measuring the degree of dissolution of formulation components when solid formulations such as tablets, granules and capsules are immersed in a solvent. The present invention relates to a test liquid injecting device that can inject a set amount of water or a chemical solution into a test container.

[Conventional technology]

In recent years, dissolution tests of solid preparations such as tablets, granules and capsules have been regarded as important as one of the methods for evaluating the quality of preparations. This dissolution test examines the dissolution rate of the main drug when the solid preparation is immersed in various solvents, and the solid preparation is poured into a test container in a predetermined amount and kept in a solvent maintained at a temperature of 37 ° C. The solution is introduced, a part of the solution is sampled a plurality of times with the passage of time, and each sample solution sampled is sequentially measured for absorbance by a spectrophotometer to record the time-dependent change in the elution amount of the main drug. In the case of simultaneously measuring multiple components in a preparation, a sample liquid is sampled and subjected to liquid chromatography analysis.

In this dissolution test method, the radius was 50 to 52.5 mm, the inner bottom surface of the semicircle was open widely at the upper end surface, and the capacity was 1,00.
A 0 ml glass container is used and 500-500
A test solution (solvent) is injected in an amount set for every 100 ml within a range of 900 ml, and the solid preparation is put into the test solution and dissolved. Here, in order to inject the test solution into the test container, conventionally, the test solution is manually weighed using a measuring cylinder or a measuring flask, and the weighed test solution is transferred from the measuring cylinder or the measuring flask to the test container. I was trying to transfer it.

Also, for example, JP-B-63-38097, JP-B-63-38097
No. 98, Japanese Unexamined Patent Publication No. 57-44853, etc., a test container and a spare container containing a test solution are arranged side by side, and the pump is operated at the beginning of the dissolution test. By doing so, a predetermined amount of the test liquid is injected from the spare container into the test container through an injection container disposed between the spare container and the test container. Alternatively, JP-A-63-196859 discloses that a test liquid is introduced into a test container from a test liquid warmer storing and storing a test liquid at an appropriate temperature by operating an electromagnetic valve. In addition, there is disclosed a fully automatic dissolution test apparatus which detects a liquid level of a test liquid by a liquid level sensor and automatically injects a predetermined amount of the test liquid into a test container.

[Problems to be solved by the invention]

However, in the method of manually weighing a test liquid into a test container using a measuring cylinder or a measuring flask, the operation is troublesome and time-consuming, and especially when the number of test containers is increased, for example, to six tanks, the work is further increased. Becomes troublesome,
In addition, weighing errors may occur.

Further, as disclosed in JP-A-63-38097, a method of operating a pump to send a test solution from a spare container to a test container and injecting a predetermined amount of the test solution into the test container requires a syringe. Use an expensive pump that can control the amount of liquid sent with high precision, such as a type pump, and properly control the number of input pulses to the pulse motor that drives the pump, so that the test solution It is necessary to carry out programming so that the injection amount of the gas is exactly as set. Therefore, there is a problem that the device configuration is complicated, the cost is high, and the programming operation is dangerous.

On the other hand, as disclosed in JP-A-63-196859, a method for adjusting the injection amount of a test solution into a test container to a constant amount by combining a solenoid valve and a liquid level sensor is not practical. In order to perform accurate liquid volume control, a special liquid volume level sensor with high detection accuracy is required. In a device with multiple test vessels, a liquid volume level sensor and solenoid valve are provided for each test vessel. It is necessary to provide a drive control mechanism for that. In addition, when the liquid level is detected by the liquid level sensor, the liquid level undulates with the injection of the test liquid into the test container, which makes accurate liquid level detection difficult. In order to prevent the surface from being ruffled, the test solution may be gently poured into the test container at a low flow rate. However, there is a problem that the operation of injecting the test solution takes time.

SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and in order to automate the operation of injecting a test solution into a test container, a conventionally expensive pump and a complicated control mechanism for controlling its drive are conventionally used. It is a technical task to automate the process without using a solenoid valve or a liquid level sensor for adjusting the injection volume without requiring the use of a test container. Liquid can be injected accurately and quickly, with a relatively simple configuration,
It is an object of the present invention to provide an apparatus for injecting a test liquid into a test container which is not so expensive in terms of cost.

[Means for solving the problem]

The present invention provides a means for achieving the above object,
A test liquid injection means for supplying a test liquid by a predetermined amount larger than a set amount to the test container, a suction nozzle whose lower end suction port enters the test container and is supported so as to be able to move up and down in the test container. A nozzle drive mechanism for moving, a vacuum suction means connected to the suction nozzle in a flow path, a control means for controlling the operations of the nozzle drive mechanism and the vacuum suction means, and a cleaning liquid supply for supplying a predetermined amount of the cleaning liquid to the test container. The gist of the present invention is that an apparatus for injecting a test liquid into a test container is configured from the means. Then, the vacuum suction means can suck the test liquid from near the liquid surface together with air through the lower end suction port with the lowering operation of the suction nozzle,
The control unit controls the nozzle driving mechanism to lower the suction nozzle to a position corresponding to the set amount of the test liquid and stop the suction nozzle.

The vacuum suction means is an airtightly sealed waste liquid tank, a suction pipe for communicating the waste liquid tank with the suction nozzle, and a suction control valve inserted in the middle of the suction pipe.
A vacuum pump connected to the waste liquid tank via a vacuum pipe, a pressure release valve attached to the waste liquid tank to open the inside of the waste liquid tank to the atmosphere, and a test attached to the waste liquid tank and remaining in the waste liquid tank And a discharge valve for discharging the liquid.

[Action]

In the apparatus for injecting test liquid into the test container having the above configuration,
First, a test liquid is injected into the test container by the test liquid injection means by a predetermined amount larger than the set amount, and the test container is filled with the test liquid. Subsequently, the nozzle driving mechanism is controlled by the control means, and the suction nozzle is lowered by the nozzle driving mechanism. When the lower end suction port of the suction nozzle enters the test container and the lower end suction port descends to the vicinity of the liquid level of the test liquid, the vacuum suction force of the vacuum suction means causes the suction nozzle connected to the suction nozzle to close the liquid level. Is sucked from the lower end suction port together with air. Then, as the suction nozzle descends, 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 the test liquid, the nozzle driving mechanism is controlled by the control means, and the descending operation of the suction nozzle is stopped. At this point, a set amount of test liquid will remain in the test container.

As described above, in this test liquid injection device, first, after filling the test container with the approximate amount of the test liquid larger than the set amount, the test liquid in excess of the set amount is discharged from the test container. Since a set amount of test liquid determined by the descent stop position of the suction nozzle is finally left in the test container, control of the amount of liquid sent by the test liquid injection means does not require very high precision. Further, a liquid level sensor and a solenoid valve for controlling the liquid amount are unnecessary, and even when a plurality of test containers are arranged in parallel in the dissolution test apparatus, a plurality of suction nozzles provided for each test container are required. Are connected together,
If the plurality of suction nozzles are moved up and down integrally by a common nozzle drive mechanism, it is not necessary to control the liquid amount for each test container. In this test liquid injection device, the test liquid is injected into the test container at a stretch by the test liquid injection means, and then the suction nozzle is lowered at an appropriate speed. Since the liquid is injected, the injection operation of the test liquid is completed in a short time. Further, since the cleaning liquid supply means for supplying a predetermined amount of the cleaning liquid to the test container is provided, the cleaning operation of the test container can be automatically performed.

〔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 configuration diagram of a device for injecting a test solution into a test container, which constitutes a part of a dissolution test device. FIG. 2 is a dissolution device of the dissolution test device. It is the longitudinal section which looked at a part from the front direction. In FIG. 2, a drive mechanism of a paddle (stirring blade) which is not directly related to the present invention is not shown.

First, the configuration of the elution device will be described with reference to FIG. The dissolution apparatus is provided with a constant temperature water bath 10 made of transparent glass filled with constant temperature water adjusted to 37 ° C. In this constant temperature water bath 10, in this embodiment, six round-bottomed test vessels are provided. 12 is fitted by inserting the whole body of the test container 12 almost through the circular opening 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 portion of the circular opening, respectively. I have. And each test container
The upper end opening surfaces of 12 are closed by lids 14, respectively. The lid 14 is formed with a groove-like hole 16 cut from the periphery to a position corresponding to the center position of the upper end opening surface of each test container 12. A shaft 22 (only a part thereof is formed) integrally formed with a stirring blade 20 at the lower end thereof is suspended through each groove-shaped hole 16 of the lid 14.
Is connected to a rotation drive mechanism (not shown). Further, suction nozzles 24 are respectively hung down through the respective groove-shaped holes 16 of the lid 14. A sampling hole 26 is further formed in the lid 14, and the sampling nozzle 28 is lowered through the sampling hole 26 to
Thereby, a part of the eluate in the test container 12 can be collected and sent to an analyzer (not shown) such as a spectrophotometer. In addition, a test liquid injection nozzle 30 and a pair of cleaning liquid supply nozzles 32, 32 are disposed at the upper end opening of the test container 12 so as to face each test container 12.

Each of the six suction nozzles 24 is fixed to one connecting plate 34 at the upper end, and the six suction nozzles
24 ascends and descends integrally. Also, connecting plate
3, is fixedly supported by a U-shaped support plate 36, as shown in FIG. On the support plate 36, a nut member 38 and a pair of bearing members 40, 40 are integrally fixed. The nut member 38 is screwed to the threaded rod 24 held in the vertical position, and is coupled to the pair of bearing members 40, 40, and to the respective guide rods 44, 44 held in parallel to the threaded rod 42. A pair of guide rods 44, 44 are slidably engaged with each other by driving a drive motor 46 having a lower end of the screw rod 42 and a rotating shaft connected thereto to rotate the screw rod 42 forward and reverse. The support plate 36 is moved up and down while being guided by the guide plate, and accordingly, the six suction nozzles 24 fixed to the connecting plate 34 are simultaneously moved up and down. In FIG. 3, the portion where the guide rod 44 is fixed to the device fixing portion is not shown, and the stirring blade, the constant temperature water tank, the lid, etc. are also not shown, and the nozzle is not shown. The configuration of the drive mechanism is made easy to understand.

Next, a configuration other than the above in the test liquid injection device will be described based on FIG. The suction nozzle 24 communicates with the airtightly sealed internal space of the waste liquid tank 50 via a suction pipe 48 connected to the suction nozzle 24, and a suction control valve 52 is inserted in the suction pipe 48. And the waste tank
50 is connected to a vacuum pump 56 via a vacuum pipe 54. Further, the waste liquid tank 50 is provided with a pressure control valve 58 for opening the inside of the waste liquid tank 50 to the atmosphere, and a drain pipe 60 for discharging the liquid remaining in the waste liquid tank 50. The drain valve 60 is provided in the drain pipe 60.

The test liquid injection nozzle 30 is connected to a test liquid tank 68 storing the test liquid 66 through an injection pipe 64 connected to the test liquid injection nozzle 30.
And an injection control valve 72 are interposed respectively. The test liquid 66 in the test liquid tank 68 is kept at about 37 ° C.
Further, the cleaning liquid supply nozzle 32 is connected to a cleaning liquid tank 78 in which the cleaning liquid 76 is stored through a liquid transmission pipe 74 connected thereto, and a liquid supply pump is provided in the middle of the liquid transmission pipe 74.
80 and a liquid sending control valve 82 are inserted respectively. Then, while controlling the nozzle drive mechanism 84 for vertically moving the suction nozzle 24, driving and stopping each of the pumps 56, 70, 80,
In addition, a control device (microcomputer) 86 for controlling opening and closing of various control valves 52, 58, 62, 72, 82 is provided. Note that reference numerals 88 and 90 in the figure denote liquid level sensors disposed in the waste liquid tank 50.

Next, the operation of the test liquid injection device configured as described above will be described with reference to FIG. In FIG. 4, the lid and the like of the test container 12 are not shown.

First, as shown in FIG. 4 (a), in a state where the suction nozzle 24 is kept at the upper position, the injection pump 70 is driven by a control signal from the control device 86, and the injection control valve is controlled.
By opening 72, 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. (B), the control device is previously controlled by a keyboard.
The amount set to 86, for example, 5 from the set amount of 600 ml
After the test liquid 66 is injected into the test container 12 in an amount larger by about 0 ml, the injection pump 70 is stopped and the injection control valve 72 is closed. Next, the vacuum pump 56 is driven, and the suction control valve 52 is
Then, the suction nozzle 24 is lowered at a high speed by the nozzle drive mechanism 84, and the lower end suction port 92 of the suction nozzle 24 is advanced into the test container 12, and as shown in FIG. When the lower end suction port 92 of the suction nozzle 24 descends to near the liquid level of the test liquid 66, the descent speed of the suction nozzle 24 is reduced. At this time, the test liquid 66 near the liquid surface is sucked into the suction nozzle 24 together with air from the lower end suction port 92 by the vacuum suction force of the vacuum pump 56, and subsequently, from the inside of the test container 12 according to the lowering operation of the suction nozzle 24. The test liquid 66 is discharged through the suction nozzle 24 at a speed of, for example, about 10 ml / sec.
The amount of the test liquid 66 in the inside gradually approaches the set amount. The test liquid and air sucked into the suction nozzle 24 are:
The test liquid flows into the waste liquid tank 50 through the suction pipe 48, and the air therein is exhausted through the vacuum pipe 54 and the vacuum pump 56, and the test liquid accumulates in the waste liquid tank 50. Then, as shown in FIG. 4 (d), the lower end suction port of the suction nozzle 24
When 92 falls to a position corresponding to the set amount, the control device 86
The nozzle driving mechanism 84 is controlled by the signal from the controller to stop the lowering operation of the suction nozzle 24, and then the suction nozzle 24
Rises and returns to the original upper position shown in FIG. 4 (e). In this way, the set amount of the test liquid 66 determined by the descent stop position of the suction nozzle 24 finally remains in the test container 12, and the injection operation of the test liquid is completed. And finally,
The test liquid collected in the waste liquid tank 50 is discarded through the drain pipe 60 by opening the pressure control valve 58 to set the inside of the waste liquid tank 50 to atmospheric pressure, and then opening the discharge valve 62, or discarded or reused. Offer.

In addition, the above-described liquid amount adjustment operation shown in FIGS. 4B to 4E is performed by integrally operating the suction nozzles 24 for six (three in some cases) test containers 12. Done at the same time. FIG. 5 shows a flowchart of the above-described series of test liquid injection operations.

The above is the description of the configuration and the operation of the apparatus for injecting a test liquid into a test container. According to this embodiment, the operation of cleaning the test container can be performed automatically. Sixth
The operation of cleaning the test container will be described based on the drawings.

First, as shown in FIG. 6 (a), with the suction nozzle 24 standing by at the upper position, the controller 86 drives the liquid feed pump 80 and opens the liquid feed control valve 82,
The cleaning liquid 76 is sent from the cleaning liquid tank 78 to the test container 12 through the liquid supply pipe 74, and the cleaning liquid 76 is jetted from the cleaning liquid supply nozzle 32 into the test container 12 in a conical shape. At this time, the cleaning liquid 76 is sprayed on the inner wall surface of the test container 12, flows down while wetting the entire inner wall surface, 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 signal from the control device 86 is received, the liquid supply pump 80 is stopped, and the liquid is supplied. The control valve 82 is closed, and the supply of the cleaning liquid 76 is stopped. Next, after driving the vacuum pump 56 and opening the suction control valve 52, the suction nozzle 24 is moved by the nozzle driving mechanism 84, and the lower end suction port 92 enters the inside of the test container 12, and the vicinity of the inner bottom surface of the test container 12. And then stop at a constant speed until it reaches. In the process of lowering the suction nozzle 24, as shown in FIG. 6C, 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 discharged from the test container 12. At this time, the cleaning liquid and air sucked into the suction nozzle 24
The air flows into the waste liquid tank 50 through the suction pipe 48, the air is exhausted through the vacuum pipe 54, and the cleaning liquid is stored in the waste liquid tank 50. Finally, the suction nozzle 24 moves up, returns to the original upper position shown in FIG. 6 (e), and one cleaning operation is completed. Then, if necessary, the above series of cleaning operations are repeated several times. Then, the cleaning liquid accumulated in the waste liquid tank 50 is discarded through the drain pipe 60 by opening the pressure control valve 58 to make the inside of the waste liquid tank 50 atmospheric pressure, and then opening the discharge valve 62.

Although the apparatus for injecting a test solution into a test container of the present invention has the above-described configuration, the scope of the present invention is not limited by the above description and the contents of the drawings, and does not depart from the gist. Various modifications may be included. That is, the configurations of the test liquid injection unit, the nozzle driving mechanism, the vacuum suction unit, and the like are not limited to those of the above-described embodiment.

〔The invention's effect〕

Since the present invention is configured and operates as described above, according to the present invention, it is possible to automatically and accurately inject a test liquid in a test container in a set amount exactly, and the device configuration is relatively simple, and the control is relatively simple. The mechanism was not so complicated, the cost was not so high, and a device for injecting a test solution into a test container suitable for use in a dissolution test device or the like could be provided.

[Brief description of the drawings]

FIG. 1 is a schematic configuration diagram of an apparatus for injecting a test solution into a test container according to one embodiment of the present invention. FIG. 2 is a longitudinal sectional view of a dissolution apparatus section of the dissolution test apparatus viewed from the front. FIG. 4 is a perspective view showing an example of the configuration of the nozzle drive mechanism. FIG. 4 is a vertical sectional side view for explaining a series of operations in the test liquid injection device. FIG. 5 is a series of test liquid injection operations. FIG. 6 is a vertical sectional side view for explaining the cleaning operation of the test container by the apparatus of the above embodiment. 12 ... test container, 24 ... suction nozzle, 30 ... test liquid injection nozzle, 32 ... cleaning liquid supply nozzle, 34 ... connecting plate, 36 ... support plate, 38 ... nut member, 40 ... bearing member , 42… screw rod, 44… guide rod, 46… drive motor, 48… suction pipe, 50… waste liquid tank, 52… suction control valve, 54… vacuum pipe, 56… vacuum pump, 58 …… Pressure control valve, 60 …… Drain pipe, 62 …… Discharge valve, 64 …… Injection pipe, 66 …… Test liquid, 68 …… Test liquid tank, 70 …… Injection pump, 72 …… Injection control valve , 74… Liquid supply piping, 76… Cleaning liquid, 78… Cleaning liquid tank, 80… Liquid supply pump, 82… Liquid supply control valve, 84… Nozzle drive mechanism, 86… Control device, 92… Lower end suction port.

──────────────────────────────────────────────────続 き Continued on front page (58) Field surveyed (Int.Cl. ⁷ , DB name) G01N 35/00-35/10

Claims (2)

(57) [Claims] 1. A test liquid injecting means for injecting a test liquid by a predetermined amount larger than a set amount into a test container, a suction nozzle having a lower end suction port which enters into the test container and is supported so as to be vertically movable in the test container; A nozzle drive mechanism for moving the suction nozzle up and down, a flow path connected to the suction nozzle, and a vacuum suction means for sucking a test liquid from near the liquid surface together with air through the lower end suction port as the suction nozzle descends, Control means for controlling the nozzle driving mechanism so as to lower the suction nozzle to a position corresponding to the set amount of test liquid and to stop the suction nozzle, and for controlling operation of the vacuum suction means; and supplying a predetermined amount of cleaning liquid to the test container. An apparatus for injecting a test liquid into a test container, comprising: 2. A waste liquid tank hermetically sealed, a suction pipe for communicating the waste liquid tank with a suction nozzle, a suction control valve inserted in the middle of the suction pipe, and the waste liquid. A vacuum pump connected to the tank via a vacuum pipe, a pressure release valve attached to the waste liquid tank to open the inside of the waste liquid tank to the atmosphere, and a test liquid attached to the waste liquid tank and remaining in the waste liquid tank. The apparatus for injecting a test liquid into a test container according to claim 1, further comprising a discharge valve for discharging the test liquid.