JP2006007083A - Automatic solid-phase extraction apparatus - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an automatic solid-phase extraction apparatus enabling a secure visual observation of the state where a liquid is vacuum-suctioned from a vessel with a filter. <P>SOLUTION: In the automatic solid-phase extraction apparatus which is provided with a dispensation head enabling a suction and discharging action of a liquid, a moving means moving the dispensation head, and a control means to control the suction and discharging action of the dispensation head, and the movement of the dispensation head by the moving means, and acts according to the operation process input by the control means, a temporary stop setting function stopping temporarily an action of the apparatus in advance in an arbitrary operation process is provided on the control means. More concretely, a vacuum suction means in which the inside is made vacuum and the liquid is vacuum-suctioned from the vessel with the filter is provided, and when the apparatus is in a temporary stopping state in the previously set operation process, the vacuum suction means is operated independently, and the vacuum-suctioned condition of the liquid from the vessel with the filter is confirmed by the visual observation. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to an automatic solid-phase extraction apparatus for automatically performing a solid-phase extraction operation as a pretreatment operation for analysis of organic chemical substances contained in pharmaceuticals, agricultural chemicals, water and the like.

  For example, liquid chromatography analysis is known as an analysis method for organic chemical substances contained in sample solutions of pharmaceuticals and agricultural chemicals. This analysis requires a solid-phase extraction operation as a pretreatment operation. This solid-phase extraction operation is carried out on a long cylindrical solid-phase extraction tube (column) packed with an adsorbent serving as a stationary phase. After the sample solution is dropped from the solute, the solute is adsorbed on the stationary phase, and then the solvent is flowed to separate the solute adsorbed on the stationary phase and dissolve the target component.

  Thus, in liquid chromatography analysis, after the solid phase extraction operation is performed, component analysis is performed by subjecting the solution containing the target component to liquid chromatography.

  However, solid-phase extraction operations as pretreatment operations generally require a long time, and manual operations are inefficient. In recent years, these pretreatment operations are automatically performed in order to improve the efficiency of the treatment. An automatic solid-phase extraction apparatus has been proposed.

  For example, in Patent Document 1, a head equipped with a multi-continuous needle holder for solution injection is moved to a predetermined test tube position and a flow rate control pump is operated, whereby a predetermined solvent is supplied from a solvent supply source to a plurality of solid phases. An automatic solid-phase extraction device has been proposed in which the fixed layer of each solid-phase extraction tube is simultaneously injected into the extraction tube and the activation process is performed. Can significantly reduce the processing time.

JP-A-8-164302

  However, in the conventional automatic solid phase extraction apparatus, it is impossible to detect whether or not the liquid is reliably sucked in vacuum from a solid phase extraction tube (hereinafter referred to as a container with a filter).

  By the way, it is generally known that a container with a filter is composed of a plurality of (for example, 96) wells, and the time required for vacuum suction differs depending on the concentration and type of organic chemical components. Thorough examination is necessary.

  In addition, when performing solid phase extraction, it is common to perform vacuum suction multiple times after the reagent is discharged to the filter-equipped container, so that liquid remains in the well of the filter-equipped container without vacuum suction. In spite of being in a state, if another reagent is newly injected, there is a problem that the liquid overflows from the container with the filter.

  Thus, as described above, when the vacuum suction of the liquid from the filter-equipped container is insufficient, the conventional automatic solid-phase extraction apparatus stops the operation of the apparatus by a stop signal from the control apparatus. It is easy to avoid problems, but the experimenter must monitor the apparatus, and the merit of automation cannot be obtained.

  Accordingly, the object of the present invention is to make it possible to visually set the state in which the liquid is sucked from the container with the filter by enabling the apparatus to be set in advance so that the operation of the apparatus is temporarily stopped when the vacuum suction work is finished. It is an object of the present invention to provide an automatic solid phase extraction apparatus that can be observed.

  In addition, not only solid phase extraction but also the operation of sucking and discharging liquids is generally performed. However, when dispensing a plurality of liquids, for example, the first reagent dispensing amount is 100 μl, the second time There are cases where a series of operations in which the dispensing amount is greatly different each time is required, such as 5 μl for the reagent and 1000 μl for the third reagent. In general, when 5 μl of liquid is dispensed using a dispensing head capable of dispensing 1000 μl of liquid at a time, the accuracy and reproducibility representing the accuracy of the dispenser deteriorate.

  Therefore, a dispensing head for small volume dispensing and a dispensing head for large volume dispensing are prepared, and two robot arms are used for different dispensing heads depending on the application. A method of providing a mechanism that can attach and detach the dispensing head to the tip of one robot arm has been implemented.

  However, in such a method, although all the steps can be performed fully automatically, for example, even when a series of steps require more than one hour, only a small number of small-volume dispensing heads are required. Only the portion is used, so the merit that corresponds to the investment cost cannot be obtained. Needless to say, it is necessary to prepare a small-volume dispensing tip, a reagent, and the like in addition to the small-volume dispensing head, and the apparatus becomes large and expensive.

  On the other hand, when the dispensing amount greatly exceeds the upper limit of the setting range of the dispensing head, it is necessary to repeat the dispensing operation by the dispensing head a plurality of times, resulting in a problem that the operation time becomes longer.

  Accordingly, another object of the present invention is to dispose a small volume (for example, 5 μl) or a large volume (for example, 5000 μl) outside the set range (for example, 50 to 1000 μl) of the dispensing head. Can be set in advance to temporarily stop the operation, and small-sized or large-volume dispensing is performed by a single operation using a manual method (manual operation), thereby reducing the size and cost. An object of the present invention is to provide an automatic solid-phase extraction apparatus capable of

  In order to achieve the above object, the invention according to claim 1 is a dispensing head capable of sucking and discharging a liquid, a transfer means for moving the dispensing head, and a suction and discharge of the dispensing head. In an automatic solid-phase extraction apparatus that includes a control means for controlling the operation and movement of the dispensing head by the transfer means, and that operates according to the operation process input from the control means, the operation of the apparatus is performed in an arbitrary operation process in advance. A temporary stop setting function for temporarily stopping is provided in the control means.

  The invention described in claim 2 is characterized in that, in the invention described in claim 1, a function of notifying that the apparatus is in a paused state is provided in a preset operation process.

  The invention according to claim 3 is the invention according to claim 1 or 2, wherein a container for sucking and discharging a liquid to a dispensing tip attached to the dispensing head, and a container with a filter for discharging the liquid, A vacuum suction means for vacuum suction of the liquid from the filter-equipped container with the inside being in a vacuum state, and when the apparatus is in a temporarily stopped state in a preset operation process, the vacuum suction means is operated alone to The vacuum suction state of the liquid from the filter-equipped container is visually confirmed.

  According to a fourth aspect of the present invention, in the third aspect of the present invention, the vacuum suction means removes liquid from the filter-equipped container based on the time during which the vacuum suction means is operated alone when the apparatus is in a suspended state. The vacuum suction time can be changed.

  According to a fifth aspect of the present invention, in the first or second aspect of the present invention, the apparatus includes a container for sucking and discharging a liquid to the dispensing tip mounted on the dispensing head, and the apparatus is set in a preset operation process. When the liquid is in a paused state, the liquid is dispensed into the container by a conventional method.

  The invention according to claim 6 is the invention according to any one of claims 1 to 5, wherein when no operation is performed from the control means when the apparatus is in a paused state, the apparatus is paused after a predetermined time has elapsed. The operation after the state is continued.

  A seventh aspect of the invention is characterized in that, in the sixth aspect of the invention, the predetermined time can be set from the control means.

  According to the first aspect of the present invention, the operation of the apparatus is temporarily stopped in an arbitrary operation process to interrupt the automatic operation, and during that time operation by a person is enabled. Visual confirmation and small volume dispensing by the use method become possible.

  According to the invention described in claim 2, the experimenter can know that the apparatus is in a paused state in a preset operation process.

  According to the third aspect of the present invention, the vacuum suction means is operated alone in a state in which the apparatus is temporarily stopped in the preset operation process, and the vacuum suction state of the liquid from the container with the filter is visually confirmed. Can be confirmed.

  According to the fourth aspect of the present invention, the operation time of the vacuum suction means necessary for completely vacuuming the liquid from the filter-equipped container can be reset based on the single operation time when the operation is stopped.

  According to the fifth aspect of the present invention, for example, when it is desired to dispense a small volume or a large volume outside the setting range of the dispensing head, the apparatus is temporarily stopped, and a small volume or a large volume is dispensed by a method. Since it can be performed by one operation, the apparatus can be reduced in size and cost can be reduced.

  According to the sixth aspect of the present invention, if no operation is performed for a certain period of time when the apparatus is in the paused state, the operation after the paused state is continued, so that the reagent evaporation And the occurrence of problems such as a decrease in activity level can be prevented.

  According to the seventh aspect of the present invention, the maximum time (a certain time) during which the apparatus is temporarily stopped can be arbitrarily set by the control means according to the type of liquid to be handled.

  Embodiments of the present invention will be described below with reference to the accompanying drawings.

  FIG. 1 is a perspective view of an automatic solid phase extraction apparatus according to the present invention, and FIG. 2 is a perspective view showing details of the configuration in the automatic solid phase extraction apparatus.

  An automatic solid-phase extraction apparatus 1 shown in FIG. 1 includes an apparatus main body 2, a vacuum controller 15 having a vacuum pump (not shown), and a control device 3 that controls these. Here, the control device 3 is constituted by a general-purpose personal computer, for example, and is electrically connected to the device main body 2 and the vacuum controller 15 via a communication cable 4 such as a LAN (Local Area Network).

  Further, the apparatus main body 2 includes a robot 5 which is a transfer means capable of moving and positioning in a three-dimensional space, a dispensing head 6 provided at the tip of the robot 5, and conditions input to the control apparatus 3. A circuit section (not shown) for driving the apparatus main body 2 based on the above is provided. Here, the robot 5 can move in a three-dimensional space along the X-axis-Y-axis-Z-axis that is an orthogonal coordinate axis, is driven by a stepping motor (not shown), and is positioned at a predetermined position. It should be noted that any other means such as a servo motor can be used as a drive source for the robot 5.

  The dispensing head 6 can attach and detach a plurality of dispensing tips 8 arranged in a line, and by attaching the dispensing tips 8 thereto, the liquid can be sucked and discharged. That is, for example, by attaching 12 dispensing tips 8 to the dispensing head 6 and driving 12 series of syringes (not shown) by one stepping motor, the liquid suction operation to the dispensing tips 8 and The liquid discharging operation from the dispensing tip 8 is executed. In addition, the space | interval of each syringe is set to the same 9 mm pitch as the well space | interval of the container 11 with a filter.

  Also, below the movable range of the dispensing head 6 attached to the robot 5, there are two sets of dispensing tip containers 9, four plate container groups 10, a container 11 with a filter and a carrier 12 for holding it, a vacuum container 13 and a disposal container 14 for disposing of the dispensing tip 8 that is no longer required after being used for dispensing the reagent.

  In each of the dispensing tip containers 9, a total of 96 dispensing tips 8 of 12 vertical × 8 horizontal are arranged at the same 9 mm pitch as the well interval of the container 11 with a filter. The four plate container groups 10 include reagent containers 10a and 10b containing reagents, a standard solution container 10c containing a standard solution, and a sample prepared in advance for solid-phase extraction as a pretreatment. A sample container 10d to be used is included. The reagent containers 10a and 10b are partitioned into a plurality of tanks, and a plurality of reagents are stored in these tanks. In addition, the standard solution container 10c and the sample container 10d are partitioned into a total of 96 wells of 12 vertical x 8 horizontal, and a plurality of standard solutions are accommodated in the standard solution container 10c. In 10d, a specimen (sample) to be subjected to solid phase extraction is stored in advance.

  Further, the filter-equipped container 11 is detachably attached to the carrier 12 disposed at the upper part of the vacuum container 13, and convex portions 12a and 12b projecting upward are formed on the left and right of the upper part. In the container 11 with a filter, a total of 96 wells of 8 vertical × 12 horizontal are formed in a lattice shape.

  Also, hooks 6a and 6b are attached to the left and right of the dispensing head 6 so as to be able to come into contact with the convex portions 12a and 12b of the carrier 12, and the robot 5 is moved to move the hooks 6a and 6b. The carrier 12 can be moved to the front side 13a and the back side 13b of the vacuum vessel 13 by engaging the projections 12a and 12b. As described above, the carrier 12 is moved in the front-rear direction with respect to the vacuum container 13, and in the solid-phase extraction, there are cases where the liquid vacuumed from the container 11 with the filter is necessary and unnecessary. Therefore, in the present embodiment, the front side 13a of the vacuum vessel 13 is a side that receives unnecessary liquid (referred to as a Load side), and the back side 13b is a side that receives necessary liquid (referred to as a Collect side). A collection container 13c is installed on the collect side 13b.

  Further, by moving the robot 5 and pressing the projections 12a and 12b of the carrier 12 with the hooks 6a and 6b, the lower surface of the filter-equipped container 11 mounted on the carrier 12 and the load side 13a or collect side 13b of the vacuum container 13 are obtained. And the vacuum controller 15 is driven to control the interior of the space selectively to be in a vacuum state, whereby the liquid in the filter-equipped container 11 is loaded on the load side 13a of the vacuum container 13 or Collect. Vacuum is drawn to side 13b.

  By the way, in the automatic solid-phase extraction apparatus 1 according to the present embodiment, the apparatus main body 2 is covered with the safety cover 16 so that a hand or the like cannot be put into the apparatus main body 2 during operation. When the safety cover 16 is opened during operation, the power supplied to the robot 5 is shut off and the movement of the robot 5 is stopped.

Here, an example of operation of the conventional automatic solid phase extraction apparatus will be described with reference to FIG. Since the basic configuration of the conventional automatic solid-phase apparatus is the same as that of the automatic solid-phase extraction apparatus 1 according to the present invention, the same elements as those shown in FIGS. It explains using.
[Conventional example]
FIG. 3 is a diagram showing a specific example of a conventional operation process. This conventional example is an example in which the operation is not temporarily stopped, and the process is performed through the steps 1 to 12 sequentially.

  First, an experimenter using the automatic solid-phase extraction apparatus 1 determines an operation process in advance using the control device 3 before starting the operation, and supplies necessary dispensing tips 8 and reagents from the determined operation process. They are arranged according to the arrangement screen displayed on the screen of the control device 3.

  In Step 1 shown in FIG. 3, 50 μl of MeOH (methanol) solvent previously placed in the standard solution container 10c is sucked and discharged to the sample container 10d. The process is performed according to the following procedure.

  That is, first, the robot 5 is moved, and the nozzle portion at the lower end of the dispensing head 6 is press-fitted into the upper opening portion of the dispensing tip 8 accommodated in the dispensing tip container 9, thereby causing the dispensing head 6 to move. A dispensing tip 8 is attached. Thereafter, the dispensing head 6 is moved upward to complete the mounting of the dispensing tip 8.

  Next, the dispensing head 6 is moved to a predetermined row of the standard solution container 10c containing the MeOH solvent, and the dispensing head 6 is moved to a position where the tip of the dispensing tip 8 attached thereto is immersed in the MeOH solvent. Lower. Then, a syringe (not shown) is controlled in the suction direction to suck 50 μl of MeOH solvent into the inside of the dispensing tip 8 attached to the dispensing head 6, and then the dispensing head 6 is moved upward to suck the MeOH solvent. Complete the operation.

  Next, the dispensing head 6 is moved to the designated area of the sample container 10d, and the MeOH solvent in the dispensing tip 8 is discharged to the sample container 10d by controlling the syringe in the discharge direction.

  After the MeOH solvent suction and discharge operations are repeated a specified number of times, the dispensing head 6 is moved above the waste container 14 and the dispensing tip removal mechanism (not shown) is driven to make it unnecessary. The step 1 is completed by removing the dispensing tip 8 from the dispensing head 6 and discarding it into the disposal container 14.

  Steps 2 to 6 are different from each other in the aspiration position due to different reagents, and there are differences in the dispensing amount. From the mounting of the dispensing tip 8 to the disposal of the dispensing tip 8 through the suction and discharge of the reagent. The flow of is the same as the flow of Step 1 described above.

  Next, in Step 7, first, the carrier 12 is moved to the load side 13 a of the vacuum vessel 13. Here, when the carrier 12 is not on the load side 13a, the hooks 6a and 6b of the dispensing head 6 are engaged with the convex portions 12a and 12b of the carrier 12 to move the carrier 12 to the load side 13a. In this case, in a state where the dispensing tip 8 is attached to the dispensing head 6, the dispensing tip 8 collides with the filter-equipped container 11 before the hooks 6a, 6b contact the convex portions 12a, 12b. The carrier 12 is moved before mounting the tip 8.

  As in the case of Step 1, the robot 5 is moved, and the nozzle portion at the lower end of the dispensing head 6 is press-fitted into the upper end opening of the dispensing tip 8 accommodated in the dispensing tip container 9, thereby separating the dispensing tip 6. A dispensing tip 8 is attached to the injection head 6. Thereafter, the dispensing head 6 is moved upward to complete the mounting of the dispensing tip 8.

  Next, the dispensing head 6 is moved to the row of reagent containers 10a or 10b containing the reagent MeOH to be dispensed, and the dispensing head 6 is lowered to a position where the tip of the dispensing tip 8 is immersed in MeOH. Then, a syringe (not shown) is controlled in the suction direction to suck 500 μl of MeOH into the inside of the dispensing tip 8 attached to the dispensing head 6, and then the dispensing head 6 is moved upward to perform the MeOH suction operation. Complete.

  Next, the dispensing head 6 is moved to the designated area of the filter-equipped container 11 mounted on the carrier 12 moving to the load side 13a, and the MeOH in the dispensing tip 8 is controlled by controlling the syringe in the discharge direction. Is discharged into the container 11 with a filter.

  After repeating the above-mentioned MeOH suction and discharge operations a specified number of times, the dispensing head 6 is moved above the waste container 14 and the dispensing tip removal mechanism (not shown) is driven to make dispensing unnecessary. The tip 8 is removed from the dispensing tip 6 and discarded in the waste container 14.

  Next, the robot 5 is moved and the projections 12a and 12b are pressed downward by the hooks 6a and 6b, so that the lower surface of the filter-equipped container 11 mounted in the carrier 12 on the load side 13a and the load of the vacuum container 13 are loaded. The space formed with the side 13a is sealed. From this state, the vacuum pump in the vacuum controller 15 is driven, and the sealed space is evacuated (depressurized state), and the liquid in the filter-equipped container 11 is sucked into the load side 13 a of the vacuum container 13. To do. After holding this state for 1 minute, the vacuum controller 15 stops the operation of the vacuum pump, moves the dispensing head 6 upward, and ends the step 7.

  Steps 8 to 12 are different from each other in the movement of the carrier 12, although the aspiration position (reagent container 10 a or 10 b, sample container 10 d), the dispensing amount, and the position of the container 11 with a filter (that is, the position of the carrier 12) are different. The flow from mounting the tip 8, aspirating and discharging the reagent, discarding the tip 8, pressing the convex portions 12 a and 12 b of the carrier 12, and controlling the vacuum controller 15 is the same as the flow of Step 7.

  Finally, in Step 12, the carrier 12 on which the filter-equipped container 11 is mounted is moved to the Collect side 13b side, and vacuum suction is performed on the Collect side 13b of the vacuum container 13, and the vacuum-sucked liquid is extracted as a result of solid phase extraction. It collect | recovers by the collection | recovery container 13c, and applies this liquid to a detector (for example, a differential refraction detector, an ultraviolet absorption detector, an ultraviolet spectrophotometer, a fluorometer), and analyzes a component.

  The above is the operation flow of the automatic solid-phase extraction apparatus 1.

  Next, an example of solid phase extraction operation using the automatic solid phase extraction apparatus 1 according to the present invention will be described.

  In the prior art, MeOH (methanol) is dispensed at Step 7 and H 2 O (water) is dispensed at Step 8 into the filter-equipped container 11. This operation is necessary to activate the filter-equipped container 11. At this time, since the sample (specimen) is not mixed in the filter-equipped container 11, there is no difference in the density of the dispensed solution, and vacuum suction from the filter-equipped container 11 is easy. There is almost no variation in time until the suction for each well of the container 11 is completed.

  Next, in Step 9, the liquid containing the sample is dispensed from the sample container 10d to the filter-equipped container 11, but vacuum suction at this time may be difficult to vacuum depending on the type and concentration of the sample, so be particularly careful. There is a need.

  Therefore, in the present embodiment, as in the operation process shown in FIG. 4, a temporary stop step can be set from the control device 3 to the process in which the operation is to be stopped in advance. In this embodiment, as shown in FIG. 4, “pause” is set as Step 9 ′ after the processing of “sample container 10 d → dispensing to filter-equipped container 11 on the load side 13 a → vacuum suction” in Step 9 is completed. Yes.

  When “temporary stop” is set in Step 9 ′ in this way, the automatic solid-phase extraction apparatus 1 performs operations from “Step 1 to Step 9” to “sample container 10d → dispensing to filter-equipped container 11 on load side 13a → vacuum suction”. The robot 5 is held in a stopped state.

  By the way, it is a waste of time to leave the automatic solid-phase extraction apparatus 1 in a temporarily stopped state. In addition, if the experimenter is always concerned that the automatic solid-phase extraction apparatus 1 is temporarily stopped, the meaning of automation is reduced.

  Therefore, the control device 3 displays a screen indicating that it is in a paused state, and informs the experimenter that it is in a paused state by a buzzer function. A method may be adopted in which an indicator lamp or buzzer is provided in the apparatus main body 2 to inform the experimenter that the apparatus is in a temporarily stopped state.

  FIG. 5 shows a processing flow of the automatic solid-phase extraction apparatus 1 from a temporarily stopped state to restarting operation.

  First, when the automatic solid-phase extraction apparatus 1 is in a paused state (step 51), the robot 5 is completely stopped, so no error occurs even if the safety cover 16 is opened. It is possible to work safely because the power supply to be cut off.

  Therefore, the experimenter can open the safety cover 16 (step 52) and visually confirm whether or not the liquid is sucked from the filter-equipped container 11 (step 53). When the vacuum suction of the liquid is good (when the judgment result in step 53 is OK), the safety cover 16 is closed (step 54), and the operation is restarted by a command from the control device 3 (step 55). ). In the present embodiment, after the operation is resumed, the operation of Step 10 to Step 12 is performed and the process is terminated.

  On the other hand, as a result of visual confirmation, when it is determined that the vacuum suction of the liquid is insufficient (when the determination result in step 53 is NG), the vacuum controller 15 is operated alone to perform vacuum suction ( Step 56), it is visually confirmed again whether or not the liquid is sucked from the filter-equipped container 11 (step 53), and the vacuum suction is continued until it is confirmed that the liquid is sufficiently sucked. The operation of the vacuum controller 15 is set to be possible even with the safety cover 16 opened.

  FIG. 6 shows a model of the single operation screen 60 of the vacuum controller 15.

  When the experimenter determines that the vacuum suction from the filter-equipped container 11 is insufficient in the suspended state, the experimenter starts up the single operation screen 60 on the control device 3 and selects either Load 61 or Collect 62. In the case of the temporary stop state at Step 9 ′ shown in FIG. 4, since the position of the carrier 12 is the load side 13 a, a check mark is attached to the load 61. Since the robot 5 cannot be operated when the safety cover 16 is open, the experimenter presses the convex portions 12a and 12b of the carrier 12 downward by hand and the lower surface of the filter-equipped container 11 attached to the carrier 12 on the load side 13a. The space formed on the load side 13a of the vacuum vessel 13 is sealed. In this state, when the start button 63 on the single operation screen 60 is pressed, the vacuum controller 15 drives the vacuum pump, and vacuums the liquid from the filter-equipped container 11 to the load side 13 a of the vacuum container 13.

  While the vacuum controller 15 is being operated, the operation time is displayed in the operation time display field 65. When the Stop button 64 is pressed, the vacuum controller 15 stops the operation of the vacuum pump. In this state, it is confirmed whether or not the liquid in the filter-equipped container 11 is vacuumed. If the vacuum suction state is insufficient, the same operation as described above is repeated, and it is determined that the vacuum suction state is sufficient. The safety cover 16 is closed (step 54 in FIG. 5), and the operation is restarted by a command from the control device 3 (step 55).

  In the isolated operation screen 60 shown in FIG. 6, since the time for controlling the vacuum controller 15 is displayed in the operation time display column 65, the sum of this time and the time of vacuum suction in Step 9 shown in FIG. This is the time required for vacuum suction. That is, the time required for vacuum suction is 2 minutes and 36 seconds, which is obtained by adding the time (1 minute and 36 seconds in FIG. 6) vacuumed from the single operation screen 60 to the vacuum suction time of 1 minute in Step 9. .

  Therefore, after that, if the same sample is used and the operation is performed according to the same operation process, the vacuum suction time of Step 9 should be set to 2 minutes and 36 seconds (for example, 3 minutes with a margin) instead of 1 minute. For example, the possibility that the vacuum suction state is determined to be insufficient in the visual check from the temporary stop state (step 53 in FIG. 5) is reduced.

  In the present embodiment, a temporary stop is set in advance as Step 9 ′ after the processing of “sample container 10d → dispensing to filter-equipped container 11 on load side 13a → vacuum suction” in Step 9 shown in FIG. Of course, the point for setting the pause is arbitrary, and the pause may be set after the step that the experimenter wants to confirm visually.

  The following usage method is also conceivable by setting a pause in an arbitrary process in advance.

  As in the example of the operation process shown in FIG. 3, the dispensing amount at Step 1 to Step 5 is 50 μl, whereas the dispensing amount at Step 6 to Step 12 is 500 μl or more. The automatic solid-phase extraction apparatus 1 according to the present embodiment has no problem because 50 μl to 1000 μl can be dispensed with only one dispensing head 6 and one kind of dispensing tip 8.

  However, depending on the content of the experiment, a few μl of liquid may have to be performed as a series of operations. For example, a case like the operation process example shown in FIG. 7 will be described.

  The operation process example shown in FIG. 7 is different from the operation process example shown in FIG. 3 in that the dispensing amount of the internal standard solution of Step 5 is 5 μl. As described above, since the dispensing range in the automatic solid-phase extraction apparatus 1 according to the embodiment of the present invention is 50 μl to 1000 μl, the apparatus 1 cannot be operated. In this case, a small-capacity and large-capacity dispensing head 6 and a dispensing tip 8 are incorporated in the apparatus, respectively, and mounted on two robots 5 for control, or one robot 5 has a small-capacity and large-capacity 2 It is conceivable to adopt a structure in which a kind of dispensing head 6 is detachable. As described above, any of these methods leads to an increase in size and cost of the apparatus.

  Therefore, in the above case, Step 5 may be set as a temporary stop as in the example of the operation process shown in FIG. In this case, when the automatic solid-phase extraction apparatus 1 is temporarily stopped at Step 5, the experimenter opens the safety cover 16, dispenses 5 μl of the internal standard solution into the sample container 10d by the method, and closes the safety cover 16. Thus, the operation can be resumed from the control device 3.

  In this embodiment, an example has been described in which a small volume (5 μl) whose dispensing volume is below the lower limit (50 μl) of the setting range (50 μl to 1000 μl) of the dispensing head 6 is dispensed by a method (manual operation). However, even if the dispensing volume is, for example, 5000 μl, which greatly exceeds the upper limit (1000 μl) of the setting range of the dispensing head 6, the operation of the apparatus is temporarily stopped, and the operation (manual operation) can be performed once. Large-volume dispensing can be performed, and it is not necessary to repeat the dispensing operation by the dispensing head 6 a plurality of times, and the working time can be shortened.

  The temporary stop function of the present embodiment is characterized in that the experimenter can perform some operation from the control device 3 in the temporary stop state in the operation process example shown in FIG. 4 or the operation process example shown in FIG. .

  However, if some work is not performed at all in the paused state and time elapses, problems associated with other factors such as reagent evaporation and a decrease in activity level are induced. In addition, when used for an application such as a drug metabolism test in which time is an important factor in the operation process, the test process itself may be wasted if left unnecessarily in a paused state.

  Therefore, if any operation is not performed at all in spite of a certain period of time in the paused state, it is possible to automatically continue the operation process after the pause. . In this case, when setting the temporary stop state from the control device 3, a means for setting whether or not to provide the fixed time is provided, and when the fixed time is provided, the time can be set by setting the time. Occurrence can be prevented. That is, the maximum time (a fixed time) during which the apparatus is temporarily stopped can be arbitrarily set by the control device 3 according to the type of liquid to be handled. If a certain period of time is not provided, the experimenter holds the paused state until the operation is continued.

  The present invention is useful for chemical component analysis in drug discovery screening, biotechnology, medical fields and the like.

1 is a perspective view of an automatic solid phase extraction apparatus according to the present invention. It is a perspective view which shows the detail of the structure in the automatic solid-phase extraction apparatus which concerns on this invention. It is a figure which shows the example of a solid-phase extraction operation | movement in the conventional automatic solid-phase extraction apparatus. It is a figure which shows the solid-phase extraction operation example in Example 1 of the automatic solid-phase extraction apparatus which concerns on this invention. It is a flowchart which shows the procedure from the temporary stop state in Example 1 of the automatic solid-phase extraction apparatus which concerns on this invention to a driving | operation restart. It is a figure which shows the example of a display of the independent operation screen of a vacuum controller. It is a figure which shows the solid-phase extraction operation example (when trace dispensing is required) in Example 2 of the automatic solid-phase extraction apparatus which concerns on this invention. It is a figure which shows the solid-phase extraction operation example in Example 2 of the automatic solid-phase extraction apparatus which concerns on this invention (a microdispensing is made to stop temporarily).

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Automatic solid phase extraction apparatus 2 Automatic solid phase extraction apparatus main body 3 Control apparatus (control means)
4 Communication cable 5 Robot (transfer means)
6 Dispensing head 8 Dispensing tip 9 Dispensing tip container 10 Plate container group 11 Container with filter 12 Carrier 13 Vacuum container 13a Load side vacuum container 13b Collect side vacuum container 13c Recovery container 14 Waste container 15 Vacuum controller 16 Safety cover 60 Single Operation screen 61 Load selection 62 Collect selection 63 Start button 64 Stop button 65 Operation time display field

Claims (7)

Dispensing head capable of sucking and discharging liquid, transfer means for moving the dispensing head, and controlling suction and discharge operations of the dispensing head and movement of the dispensing head by the transferring means In an automatic solid-phase extraction apparatus that operates according to the operation process input from the control means,
An automatic solid-phase extraction apparatus, wherein the control means is provided with a pause setting function for temporarily stopping the operation of the apparatus in an arbitrary operation process in advance.   The automatic solid-phase extraction apparatus according to claim 1, further comprising a function of notifying that the apparatus is in a temporarily stopped state in a preset operation process.   A container for sucking and discharging a liquid to a dispensing tip attached to the dispensing head, a container with a filter for discharging the liquid, and a vacuum for vacuum suction of the liquid from the container with the filter while the inside is in a vacuum state Including suction means, and when the apparatus is in a paused state in a preset operation process, the vacuum suction means is operated alone to visually confirm the vacuum suction state of the liquid from the container with the filter. The automatic solid-phase extraction apparatus according to claim 1 or 2, characterized in that   The time for the vacuum suction means to vacuum the liquid from the filter-equipped container can be changed based on the time when the vacuum suction means is operated independently when the apparatus is in a paused state. Item 4. The automatic solid phase extraction apparatus according to Item 3.   A dispensing tip mounted on the dispensing head is provided with a container for sucking and discharging the liquid, and when the apparatus is in a paused state in a preset operation process, the liquid is dispensed into the container by a method. The automatic solid-phase extraction apparatus according to claim 1 or 2, wherein:   The operation after the temporary stop state is continued after a certain time if no operation is performed from the control means when the device is in the temporary stop state. Automatic solid phase extraction equipment.   7. The automatic solid-phase extraction apparatus according to claim 6, wherein the predetermined time can be set from the control means.

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