WO2020174514A1

WO2020174514A1 - Analysis system

Info

Publication number: WO2020174514A1
Application number: PCT/JP2019/006952
Authority: WO
Inventors: 祐介横井
Original assignee: 株式会社島津製作所
Priority date: 2019-02-25
Filing date: 2019-02-25
Publication date: 2020-09-03
Also published as: JPWO2020174514A1; JP7095797B2

Abstract

An embodiment of an analysis system according to the present invention is an analysis system for liquid chromatography comprising: a liquid-feeding pump (2) that feeds a mobile phase; an auto-sampler (4) fluidly connected to a downstream of the liquid-feeding pump (2), for injecting a sample into the moving phase fed by the liquid-feeding pump (2); a column oven (6) that receives inside thereof a separation column (18), which is fluidly connected to a downstream of the auto-sampler (4) to separate the sample for each component, to perform temperature control of the separation column (18); and a detector (8) that comprises a sample cell (20) through which eluate from the separation column (18) is caused to flow and a light source (22) which irradiates the sample cell (20) with light and that is for detecting sample components in the eluate from the separation column (20). The analysis system for liquid chromatography comprises: an error detection unit (26) configured so as to detect an error in the analysis system; an on-error operation setting unit (28); a shutdown procedure storage unit (30) storing a procedure of the shutdown; and an on-error operation execution unit (34). The on-error operation setting unit (28) is configured so as to set, in accordance with selection by a user, on-error operation of the analysis system when the error detection unit (26) detects an error, and is configured so as to set, as the on-error operation, a shutdown that stops feeding by the liquid-feeding pump, stops the temperature control of the separation column (18) by the column oven (6), and turns off the light source (22) of the detector (8). The on-error operation execution unit (34) is configured to control the operations of the liquid-feeding pump (2), the column oven (6), and the detector (8) so as to execute the on-error operation set by the on-error operation setting unit (28) when the error detection unit (26) detects an error, and is configured so as to execute the shutdown by the procedure stored in the shutdown procedure storage unit (30) in a case where the shutdown is set as the on-error operation when the error detection unit (26) detects an error.

Description

Analysis system

The present invention relates to an analysis system for liquid chromatography.

A liquid chromatography analysis system may be equipped with a function of automatically stopping the operation of the liquid delivery pump when an error such as clogging of a pipe or poor delivery of the liquid delivery pump occurs (Patent Document 1). See 1.). On the other hand, once the light source of the detector is turned off, it takes time to stabilize the light amount after relighting, so it is generally not automatically turned off even if an error occurs. Target.

JP, 2011-099764, A

When using the analysis system for nighttime continuous tests, an error may occur when the user is absent. In such a case, if the light source of the detector is left on, the light source will be consumed more, and if the operation of the liquid feed pump is stopped in that state, the sample cell of the detector will be empty and On the other hand, light is irradiated for a long time, the sample cell becomes dirty, and the light transmittance is changed, which may adversely affect the subsequent analysis results. Further, if the liquid feed of the mobile phase by the liquid feed pump is stopped when the temperature inside the column oven is high, the separation column is overheated and left at a high temperature, and the deterioration of the packing material also progresses. Occurs.

On the other hand, if the liquid feed pump continues to operate even after an error occurs, the mobile phase will be wasted. Further, if the liquid feed pump is continuously operated in a state where the mobile phase is used up, the liquid feed pump may be damaged by idling the liquid feed pump.

The present invention has been made in view of the above problems, and it is an object of the present invention to reduce the damage received by the elements constituting the analysis system when an error occurs in the analysis system.

The analysis system according to the present invention is for injecting a sample into a mobile phase that feeds a mobile phase and a liquid phase that is fluidly connected to the downstream of the liquid feed pump and that is fed by the liquid feed pump. Of the autosampler, a separation column that is fluidly connected to the downstream of the autosampler and that separates the sample into each component is housed inside, and a column oven for controlling the temperature of the separation column, and the separation column. A sample cell for flowing an eluate from the column; and a light source for irradiating the sample cell with light, and a detector for detecting a sample component in the eluate from the separation column. An analysis system for liquid chromatography, wherein the error detection unit is configured to detect an error in the analysis system, and the analysis system of the analysis system when the error detection unit detects an error according to selection by a user. An error-time operation setting unit configured to set an error-time operation, wherein as the error-time operation, the liquid feed by the liquid feed pump is stopped, and the temperature control of the separation column by the column oven is stopped. And, an error time operation setting unit configured to be able to set a shutdown for turning off the light source of the detector, a shutdown procedure storage unit for storing the shutdown procedure, the liquid feed pump, the column oven And an error-time operation execution unit configured to control the operation of the detector and execute the error-time operation set by the error-time operation setting unit when the error detection unit detects an error. When the error detection unit detects an error, when the shutdown is set as the operation at the time of the error, the shutdown is performed by the procedure held in the shutdown procedure holding unit. And an error action execution unit.

In the analysis system according to the present invention, as an operation when an error occurs in the analysis system (operation at the time of error), at least stop of liquid transfer by the liquid transfer pump, stop of temperature control of the separation column in the column oven, and detection. Since it is configured to be able to set the shutdown including turning off the light source of the detector, the liquid feed pump is stopped, the separation column becomes hot in the column oven, and the light source of the detector remains on for a long time. This prevents the liquid delivery pump, the separation column and the light source from being damaged by the occurrence of an error. Furthermore, since the shutdown is configured to be executed according to a preset procedure, devising the procedure can further reduce the damage to each element such as the liquid feed pump and the separation column.

It is a schematic block diagram which shows one Example of an analysis system. It is a flow chart which shows the 1st procedure of shutdown at the time of an error in the example. It is a flow chart which shows the 2nd procedure of shutdown at the time of an error in the example. It is a flow chart which shows an example of operation of the example.

An embodiment of the analysis system for liquid chromatography according to the present invention will be described below with reference to the drawings.

As shown in FIG. 1, the analysis system of this embodiment includes a liquid feed pump 2, an autosampler 4, a column oven 6, a detector 8 and a controller 10.

The liquid feed pump 2 is for feeding the mobile phase. In FIG. 1, the liquid feed pump 2 is drawn so as to feed one kind of solution as a mobile phase, but it also includes one configured to be able to feed two or more kinds of solutions as a mobile phase. ..

The autosampler 4 is fluidly connected to the downstream of the liquid feed pump 2 and injects the sample into the mobile phase fed by the liquid feed pump 2. The autosampler 4 includes a needle 14 for collecting a sample from the sample container 12 and a temperature adjusting mechanism 16 for adjusting the temperature of the sample container 12 to a predetermined temperature. The needle 14 is configured to move three-dimensionally in the horizontal plane direction and the vertical direction. The temperature adjustment mechanism 16 is realized by, for example, a Peltier element that cools the rack holding the sample container 12 and a temperature sensor that detects the temperature of the rack.

The column oven 6 has a function of accommodating the separation column 18 fluidly connected to the downstream of the autosampler 4 inside and adjusting the temperature of the separation column 18 to a set temperature. Although not shown, the column oven 6 is provided with a heater for raising the internal temperature, a fan for stirring the internal space, and the like.

The detector 8 is for detecting a sample component in the eluate from the separation column 18. The detector 8 is fluidly connected to the downstream of the separation column 18 and has a sample cell 20 through which the eluate from the separation column 18 flows, a light source 22 for irradiating the sample cell 20 with light, and a sample cell An optical sensor 24 for detecting light transmitted through 20 is provided.

The control device 10 performs information communication with the liquid sending device 2, the autosampler 4, the column oven 6 and the detector 8 to operate the liquid sending device 2, the autosampler 4, the column oven 6 and the detector 8. It controls. The control device 10 is realized by a dedicated or general-purpose computer including a central processing unit (CPU) and a storage device.

The control device 10 includes an error detection unit 26, an error operation setting unit 28, a shutdown procedure storage unit 30, a cooldown time setting unit 32, and an error operation execution unit 34. The error detection unit 26, the error operation setting unit 28, the cooldown time setting unit 32, and the error operation execution unit 34 are functions realized by the CPU of the control device 10 executing a program, and the shutdown procedure storage unit. Reference numeral 30 is a function realized by a partial storage area of the storage device of the control device 10.

The error detection unit 26 is configured to detect the occurrence of an error in the analysis system based on various signals from the liquid feed pump 2, the autosampler 4, the column oven 6 and the detector 8. For example, although not shown in the drawings, the liquid feed pump 2 is equipped with a pressure sensor that detects the liquid feed pressure, and the error detection unit 26 uses the signal from the pressure sensor to cause clogging in the flow path and liquid feed. Defective delivery of the pump 2 is detected as an error. In addition, the error detection unit 26 detects liquid leaks in the autosampler 4, the column oven 6 and the detector 8, abnormal temperature of the temperature adjustment mechanism 16 of the automatic sampler 4, abnormal temperature of the inside of the column oven 6 and the like as errors. ..

The error-time operation setting unit 28 is configured to set the operation of the analysis system (hereinafter, error-time operation) when the above-described error is detected by the error detection unit 26 according to the selection by the user. As an error action that can be set, the operation of the liquid delivery pump 2 is stopped, and the needle 14 is moved to a predetermined standby position that is set so that the tip of the needle 14 of the autosampler 4 does not come into contact with any port, At least shutdown for stopping the temperature adjusting operation of the column oven 6 (that is, turning off the heater) and turning off the light source 22 of the detector 8 is included. In addition, the error operation that may be set may include a standby operation in which the liquid feed pump 2 is operated at a low speed (for example, half the speed at the time of analysis) while the light source 22 of the detector 8 is turned on. That is, the user can at least select the shutdown as described above as the operation of the analysis system when some error occurs in the analysis system.

Here, by including the operation of moving the needle 14 of the auto sampler 4 to a predetermined standby position in the shutdown at the time of error, the state in which the needle 14 is in contact with the port such as the injection port is maintained and the port is damaged. It is possible to prevent the needle 14 from bending.

The shutdown procedure storage unit 30 stores the procedure when shutdown is executed as an error action. What is the procedure of shutting down? What kind of procedure is to stop the operation of the liquid feed pump 2, move the needle 14 of the autosampler 4 to a predetermined standby position, stop the temperature adjusting operation of the column oven 6, and The light source 22 of No. 8 is specified. The shutdown procedure storage unit 30 stores a shutdown procedure according to the type of error detected by the error detection unit 26.

In this embodiment, as the shutdown procedure, the first procedure when an error relating to the liquid feeding pressure is detected and the second procedure when an error related to a fluid feeding pressure other than the liquid feeding pressure is detected are the shutdown procedure memory. It is stored in the unit 30. The error relating to the liquid sending pressure is an error in which the pressure detected by the pressure sensor provided in the liquid sending pump 2 becomes abnormal, and is mainly caused by clogging of the piping in the analysis system and the sending of the liquid sending pump 2. There is a liquid defect.

In the first shutdown procedure that may be executed when an error relating to the liquid transfer pressure is detected, as shown in FIG. 2, immediately after the error is detected by the error detection unit 26, the liquid transfer pump 2 is stopped. The operation is stopped (steps 101 and 102), then the temperature control of the column oven 6 is stopped, the needle 14 of the autosampler 4 is moved to a predetermined standby position, and the light source 22 of the detector 8 is turned off (step 103). ). Note that, if the temperature control function of the temperature control mechanism 16 of the autosampler 4 is turned off and left for a long time, the sample in the sample container 12 may deteriorate, so that the temperature control of the temperature control mechanism 16 is shut down even after the shutdown. The function may be configured to be maintained. Further, the user may be allowed to set whether to turn off the temperature adjustment function of the temperature adjustment mechanism 16 at the time of shutdown.

The second procedure of shutdown that may be executed when an error other than the delivery pressure is detected is, as shown in FIG. 3, after the error is detected by the error detection unit 26 (step 201). First, the temperature control of the column oven 6 is stopped, the needle 14 of the autosampler 4 is moved to a predetermined standby position, and the light source 22 of the detector 8 is turned off (step 202), after an error is detected. After the elapse of a predetermined cooldown time, the liquid feed pump 2 is stopped (steps 203 and 204). The sample remaining in the flow path of the analysis system can be discharged to the outside of the analysis system by continuing to feed the mobile phase for a predetermined cooldown time.

Return to Figure 1 and continue the explanation. The cooldown time setting unit 32 of the control device 10 is configured to set the cooldown time in the second procedure based on the information input by the user. That is, the user can arbitrarily set the above cooldown time.

The error-time operation execution unit 34 controls the operations of the liquid feed pump 2, the autosampler 4, the column oven 6, and the detector 8, and when an error is detected by the error detection unit 26, the error-time operation setting unit 28 is used. It is configured to execute the set error action. In particular, when shutdown is set as the error action, the error action execution unit 34 executes the shutdown according to the procedure stored in the shutdown procedure storage unit 30 when the error detection unit 26 detects the error. Is configured to.

The operation of the analysis system will be described using the flowchart of FIG. 4 together with FIG.

When analysis is started in the analysis system, the error detection unit 26 monitors whether or not any error has occurred until the analysis is completed (steps 301 and 302). When any error is detected by the error detection unit 26 (step 301), the error action execution unit 34 confirms the action set as the error action (step 303).
..

If shutdown is set as the operation at the time of error, it is confirmed whether the type of the error is related to the liquid sending pressure (step 304). If the type of error is related to the liquid delivery pressure, the error-time operation execution unit 34 executes shutdown according to the first procedure stored in the shutdown procedure storage unit 30 (step 305). On the other hand, when the type of error is related to something other than the liquid feeding pressure, the error action execution unit 34 executes shutdown according to the second procedure stored in the shutdown procedure storage unit 30 (step 306). ..

In this embodiment, a shutdown and a standby operation can be set as an error action. When shutdown is not set as the error action (step 303), that is, when the standby action is set as the error action, the error action execution unit 34 executes a predetermined standby operation (step 307). ). The standby operation is an operation for maintaining a state in which the analysis can be restarted immediately after the cause of the error is resolved. For example, if the error is related to the delivery pressure, the operation of the delivery pump 2 is stopped, but the light source 22 of the detector 8 is kept lit. This is because when the light source 22 is turned off, it takes time for the light amount of the light source 22 to stabilize when the analysis is restarted. When the error is related to something other than the liquid feeding pressure, the operation of the liquid feeding pump 2 is activated and the light source 22 of the detector 8 is kept turned on. However, if the liquid feed pump 2 is operated at the same speed as during analysis while the analysis is suspended, the mobile phase is wasted, so the liquid feed pump 2 is operated at a predetermined speed slower than during analysis. You may let me.

As described above, the analysis system of this embodiment is configured so that shutdown can be set as an error action when an error is detected. If shutdown is set as the operation at the time of error when performing, the liquid feed pump 2 is operated, the temperature control function of the column oven 6 is maintained, and the light source 22 of the detector 8 is maintained for a long time. Can be prevented. In addition, the said Example showed only an example of embodiment of the analysis system which concerns on this invention. The embodiment of the analysis system according to the present invention is as follows.

The embodiment of the analysis system according to the present invention comprises a liquid feed pump (2) for feeding a mobile phase and a liquid feed pump (2) which is fluidly connected to the liquid feed pump (2) and is fed by the liquid feed pump (2). An autosampler (4) for injecting a sample into a mobile phase to be liquefied, and a separation column (18) fluidly connected to the downstream side of the autosampler (4) for separating the sample into components. A column oven (6) that is housed inside to control the temperature of the separation column (18), a sample cell (20) for flowing an eluate from the separation column (18), and the sample cell For liquid chromatography, comprising a light source (22) for irradiating (20) with light, and a detector (8) for detecting a sample component in the eluate from the separation column (20). An error detection unit (26) configured to detect an error in the analysis system, and the analysis system when the error detection unit (26) detects an error according to a selection by a user. An error-time operation setting unit (28) configured to set the error-time operation, wherein as the error-time operation, the liquid supply by the liquid supply pump (2) is stopped, and the column oven (6) An error operation setting unit (28) configured to stop the temperature control of the separation column (18) and shut down the light source (22) of the detector (8). A shutdown procedure storage unit (30) for storing the shutdown procedure, operations of the liquid feed pump (2), the column oven (6) and the detector (8) are controlled, and the error detection unit (26). An error-time operation execution section (34) configured to execute the error-time operation set by the error-time operation setting section (28) when the error detection section (28) detects the error. 26) when an error is detected, the error configured to execute the shutdown according to the procedure held in the shutdown procedure holding unit (30) when the shutdown is set as the error action. The time operation execution unit (34).

In the first aspect of the above-described embodiment, the shutdown procedure storage unit (30) holds a plurality of shutdown procedures according to the type of error detected by the error detection unit, and the operation at the time of error is performed. The execution unit (34) detects the detected error when the error detection unit (26) detects an error when the shutdown is set as the error operation by the error operation setting unit (28). It is configured to execute the shutdown according to the procedure according to the type. According to this aspect, when the shutdown is executed due to the occurrence of the error, the shutdown is performed according to the procedure according to the type of the error.

In the second aspect of the above-described embodiment, the shutdown procedure storage unit (30) stops the liquid feeding by the liquid feeding pump (2) as the shutdown procedure when an error related to the liquid feeding pressure occurs. And storing the first procedure of stopping the temperature control of the separation column (18) by the column oven (6) after the light source (22) is turned off, and an error related to other than the liquid sending pressure is stored. As a procedure of the shutdown when the error occurs, the temperature control of the separation column (18) by the column oven (6) is stopped, the light source (22) is turned off, and the error detection unit (26) detects an error. A second procedure for stopping the operation of the liquid delivery pump (2) when a preset cooldown time has elapsed since the detection is stored, and the error-time operation execution unit (34) If the error detection unit (32) detects an error related to the liquid sending pressure when the shutdown is set as the error operation by the error operation setting unit (32), the first procedure is performed. The above-mentioned shutdown is carried out, and when the error detection unit detects an error related to other than the liquid feeding pressure, the shutdown is carried out in the second procedure.

In the above aspect, a cooldown time setting unit (32) configured to set the cooldown time based on information input by the user may be provided. Then, the user can arbitrarily set the cooldown time.

In the third aspect of the above-described embodiment, the autosampler (4) is provided so as to be movable three-dimensionally, and includes at least a needle (14) for collecting a sample from a sample container (12), The shutdown procedure storage unit (30) includes a step of moving the needle (14) to a predetermined standby position where the tip of the needle (14) does not come into contact with any port during the shutdown procedure. There is. This prevents the needle 14 from being in contact with any of the ports for a long time.

In the above aspect, the autosampler (4) includes a temperature adjustment mechanism (16) for adjusting the temperature of the sample container (12), and the procedure stored in the shutdown procedure storage unit (30) is The temperature adjustment mechanism (16) may be configured to continue operating even after the shutdown is completed. Then, when the analysis is interrupted for a long time due to the occurrence of an error, the temperature control function of the temperature control mechanism (16) is turned off and the temperature of the sample container (12) is changed. It is possible to prevent a situation in which the sample is altered.

In the fourth aspect of the above-described embodiment, the error-time operation setting unit (28) may set the standby operation in which the light source (22) of the detector (8) is continuously turned on as the error-time operation. The error-time operation execution unit (34) is configured to operate when the standby operation is set as the error-time operation by the error-time operation setting unit (28). Is configured to perform the standby operation when it detects an error. In this way, if an error occurs in a state where the user can immediately respond, if the standby operation is set as the operation at the time of error, it will be immediately after the problem causing the error is resolved. The analysis can be restarted.

The above first to fourth aspects can be arbitrarily combined.

2 Liquid feeding pump 4 Autosampler 6 Column oven 8 Detector 10 Control device 12 Sample container 14 Needle 16 Temperature control mechanism 18 Separation column 20 Sample cell 22 Light source 24 Optical sensor 26 Error detection unit 28 Error setting unit 30 Shutdown procedure memory Part 32 Cooldown time setting part 34 Action execution part at error

Claims

A liquid feed pump for feeding the mobile phase,
An autosampler, which is fluidly connected to the downstream of the liquid feed pump, for injecting a sample into a mobile phase fed by the liquid feed pump,
A column oven, which is fluidly connected to the downstream of the autosampler and contains a separation column for separating a sample into components, and which controls the temperature of the separation column,
A sample cell for flowing the eluate from the separation column, and a light source for irradiating the sample cell with light, and a detector for detecting a sample component in the eluate from the separation column, An analytical system for liquid chromatography comprising:
An error detector configured to detect an error in the analysis system,
An error-time operation setting unit configured to set an error-time operation of the analysis system when the error detection unit detects an error according to selection by a user, wherein the liquid-feed pump is the error-time operation. Stop the liquid feeding by, stop the temperature control of the separation column by the column oven, and an error-time operation setting unit configured to be able to set the shutdown to turn off the light source of the detector,
A shutdown procedure storage unit that stores the shutdown procedure,
It is configured to control the operations of the liquid feed pump, the column oven, and the detector, and to execute the error operation set by the error operation setting unit when the error detection unit detects an error. When the error detection unit detects an error, if the shutdown is set as the operation at the time of the error, the operation performed by the error detection unit is performed according to the procedure held in the shutdown procedure holding unit. An analysis system comprising: an on-error action executor configured to perform a shutdown.
The shutdown procedure storage unit holds a plurality of shutdown procedures according to the type of error detected by the error detection unit,
When the error detecting unit detects an error when the shutdown is set as the error operation by the error operation setting unit, the error operation executing unit responds to the detected error type. The analysis system according to claim 1, wherein the analysis system is configured to perform the shutdown in the procedure.
The shutdown procedure storage unit, as the shutdown procedure when an error related to the delivery pressure occurs, stops the delivery by the delivery pump and turns off the light source, and then uses the column oven. The first procedure for stopping the temperature control of the separation column is stored, and the temperature control of the separation column by the column oven is stopped as the shutdown procedure when an error other than the liquid feeding pressure occurs. It stores the second procedure of turning off the light source and stopping the operation of the liquid delivery pump when a preset cooldown time has elapsed after the error detection unit detects an error,
When the error detection unit detects an error related to the liquid feed pressure when the shutdown is set as the error operation by the error operation setting unit, the error operation execution unit is configured to perform the first operation. The shutdown is executed in the procedure of No. 1, and the shutdown is executed in the second procedure when the error detection unit detects an error other than the liquid sending pressure. Analytical system described in.
The analysis system according to claim 3, further comprising a cooldown time setting unit configured to set the cooldown time based on information input by a user.
The autosampler is provided so as to be movable three-dimensionally, and is provided with at least a needle for collecting a sample from a sample container,
The analysis according to claim 1, wherein the shutdown procedure storage unit includes a step of moving the needle to a predetermined standby position where the tip of the needle does not come into contact with any port during the shutdown procedure. system.
The autosampler includes a temperature adjustment mechanism for adjusting the temperature of the sample container,
The analysis system according to claim 5, wherein the procedure stored in the shutdown procedure storage unit is configured such that the temperature adjustment mechanism continues to operate even after the shutdown is completed.
The error operation setting unit is configured to set a standby operation for continuing to turn on the light source of the detector as the error operation.
When the error detection unit detects an error while the standby operation is set as the error operation by the error operation setting unit, the error operation execution unit executes the standby operation. The analysis system according to claim 1, which is configured.